Science.gov

Sample records for nano-composite cation-exchanger polypyrrole

  1. Synthesis and characterization of a novel hybrid nano composite cation exchanger poly-o-toluidine Sn(IV) tungstate: Its analytical applications as ion-selective electrode

    NASA Astrophysics Data System (ADS)

    Khan, Asif Ali; Shaheen, Shakeeba

    2013-02-01

    A novel organic-inorganic nano composite cation exchanger poly-o-toluidine Sn(IV) tungstate has been synthesized by incorporation of a polymer material into inorganic precipitate. The material is a class of hybrid ion-exchanger with good ion-exchange properties, reproducibility, stability and good selectivity for heavy metals. The physico-chemical properties of this nano composite material were characterized by using XRD, TGA, FTIR, SEM and TEM. The ion-exchange capacity, pH titrations, elution behavior and chemical stability were also carried out to study ion-exchange properties of the material. Distribution studies for various metal ions revealed that the nano composite is highly selective for Cd(II). An ion-selective membrane electrode was fabricated using this material for the determination of Cd(II) ions in solutions. The analytical utility of this electrode was established by employing it as an indicator electrode in electrometric titrations.

  2. Magnetic graphene - polystyrene sulfonic acid nano composite: A dispersive cation exchange sorbent for the enrichment of aminoalcohols and ethanolamines from environmental aqueous samples.

    PubMed

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

    2015-12-01

    Present study aimed at graphene surface modification to achieve selective analyte binding in dispersive solid phase extraction. Magnetic graphene - polystyrene sulfonic acid (MG-PSS) cation exchange nano-composite was prepared by non-covalent wrapping method. Composite was characterized by FT-IR and zeta potential. Material exhibited good dispersion in water and high exchange capacity of 1.97±0.16mMg(-1). Prepared nano-sorbent was then exploited for the cation exchange extraction and gas chromatography mass spectrometric analysis of Chemical Weapons Convention relevant aminoalcohols and ethanolamines from aqueous samples. Extraction parameters such as sorbent amount, extraction time, desorption conditions and sample pH were optimized and effect of common matrix interferences such as polyethylene glycol and metal salts was also studied. Three milligram of sorbent per mL of sample with 20min of extraction time at room temperature afforded 70-81% recoveries of the selected analytes spiked at concentration level of 1μgmL(-1). Method showed good linearity in the studied range with r(2)≥0.993. The limits of detection and limits of quantification ranged from 23 to 54ngmL(-1) and 72 to 147ngmL(-1), respectively. The relative standard deviation for intra- and inter-day precision ranged from 4.6 to 10.2% and 7.4 to 14.8% respectively. Applicability of the method to different environmental samples as well as the proficiency tests conducted by the Organization for the Prohibition of Chemical Weapons (OPCW) was also ascertained. PMID:26554296

  3. Nano-composite materials

    DOEpatents

    Lee, Se-Hee; Tracy, C. Edwin; Pitts, J. Roland

    2010-05-25

    Nano-composite materials are disclosed. An exemplary method of producing a nano-composite material may comprise co-sputtering a transition metal and a refractory metal in a reactive atmosphere. The method may also comprise co-depositing a transition metal and a refractory metal composite structure on a substrate. The method may further comprise thermally annealing the deposited transition metal and refractory metal composite structure in a reactive atmosphere.

  4. Test procedure for cation exchange chromatography

    SciTech Connect

    Cooper, T.D.

    1994-08-24

    The purpose of this test plan is to demonstrate the synthesis of inorganic antimonate ion exchangers and compare their performance against the standard organic cation exchangers. Of particular interest is the degradation rate of both inorganic and organic cation exchangers. This degradation rate will be tracked by determining the ion exchange capacity and thermal stability as a function of time, radiation dose, and chemical reaction.

  5. Cation exchange resin nanocomposites based on multi-walled carbon nanotubes

    NASA Astrophysics Data System (ADS)

    Fathy, Mahmoud; Abdel Moghny, Th.; Awad Allah, Ahmed Elsayed; Alblehy, AbdElhamid

    2014-01-01

    Carbon nanotubes (CNTs) are of great interest due to their potential applications in different fields such as water treatment and desalination. The increasing exploitation of multi-walled carbon nanotubes (MWCNTs) into many industrial processes has raised considerable concerns for environmental applications. The interactions of soluble salt with MWNCTs influence in the total salt content in saline water. In this work, we synthesized two cation exchange resins nano composites from polystyrene divinylbenzene copolymer (PSDVB) and pristine MWNCTs. The prepared compounds were characterized using infra red spectroscopy, thermal stability, X-ray diffraction, and electro scan microscope. Also, the ion capacities of prepared cation exchange resins were determined by titration. Based on the experimental results, it was found that the thermal stability of prepared nanocomposites in the presence of MWNCTs increased up to 617 °C. The X-ray of PSDVB and its sulfonated form exhibits amorphous pattern texture structure, whereas the nano composite exhibits amorphous structure with indication peak at 20° and 26° for the PSDVB and MWCNTs, respectively. The ion-exchange capacity increased from 225.6 meq/100 g to 466 mg/100 g for sulfonated PSDVB and sulfonated PSDVB MWNCTs-pristine, respectively.

  6. Ceramic Spheres From Cation Exchange Beads

    NASA Technical Reports Server (NTRS)

    Dynys, F. W.

    2003-01-01

    Porous ZrO2 and hollow TiO2 spheres were synthesized from a strong acid cation exchange resin. Spherical cation exchange beads, polystyrene based polymer, were used as a morphological-directing template. Aqueous ion exchange reaction was used to chemically bind (ZrO)(2+) ions to the polystyrene structure. The pyrolysis of the polystyrene at 600 C produces porous ZrO2 spheres with a surface area of 24 sq m/g with a mean sphere size of 42 microns. Hollow TiO2 spheres were synthesized by using the beads as a micro-reactor. A direct surface reaction - between titanium isopropoxide and the resin beads forms a hydrous TiO2 shell around the polystyrene core. The pyrolysis of the polystyrene core at 600 C produces hollow anatase spheres with a surface area of 42 sq m/g with a mean sphere size of 38 microns. The formation of ceramic spheres was studied by XRD, SEM and B.E.T. nitrogen adsorption measurements.

  7. Permeation of Water through Cation Exchange Membranes

    PubMed Central

    Lakshminarayanaiah, N.

    1967-01-01

    Water permeabilities as well as other membrane parameters, such as exchange capacity, water content, and specific conductance, have been measured for two cation exchange membranes in the H form. The conductance of membrane with low water content was less than that of the membrane with high water content. These data have been discussed in the light of an existing theory and found inadequate to explain the results in a quantitative way. Water permeability of the membranes subject to mechanical pressure was found to be higher than their isotopic water permeability, according to expectation. These data have been examined from the standpoint of thermodynamic and kinetic theories of water flow in membranes and used to estimate the average size of membrane pores. PMID:6048874

  8. CATION EXCHANGE METHOD FOR THE RECOVERY OF PROTACTINIUM

    DOEpatents

    Studier, M.H.; Sullivan, J.C.

    1959-07-14

    A cation exchange prccess is described for separating protactinium values from thorium values whereby they are initially adsorbed together from an aqueous 0.1 to 2 N hydrochloric acid on a cation exchange resin in a column. Then selectively eluting the thorium by an ammonium sulfate solution and subsequently eluting the protactinium by an oxalate solution.

  9. Nanoheterostructure Cation Exchange: Anionic Framework Conservation

    SciTech Connect

    Jain, Prashant K.; Amirav, Lilac; Aloni, Shaul; Alivisatos, A. Paul

    2010-05-11

    In ionic nanocrystals the cationic sub-lattice can be replaced with a different metal ion via a fast, simple, and reversible place-exchange, allowing post-synthetic modification of the composition of the nanocrystal, while preserving its size and shape. Here, we demonstrate for the first time that during such an exchange, the anionic framework of the crystal is preserved. When applied to nanoheterostructures, this phenomenon ensures that compositional interfaces within the heterostructure are conserved throughout the transformation. For instance, a morphology composed of a CdSe nanocrystal embedded in a CdS rod (CdSe/CdS) was exchanged to a PbSe/PbS nanorod via a Cu2Se/Cu2S structure. During every exchange cycle, the seed size and position within the nanorod were preserved, as evident by excitonic features, Z-contrast imaging, and elemental line-scans. Anionic framework conservation extends the domain of cation exchange to the design of more complex and unique nanostructures.

  10. Cation exchange properties of zeolites in hyper alkaline aqueous media.

    PubMed

    Van Tendeloo, Leen; de Blochouse, Benny; Dom, Dirk; Vancluysen, Jacqueline; Snellings, Ruben; Martens, Johan A; Kirschhock, Christine E A; Maes, André; Breynaert, Eric

    2015-02-01

    Construction of multibarrier concrete based waste disposal sites and management of alkaline mine drainage water requires cation exchangers combining excellent sorption properties with a high stability and predictable performance in hyper alkaline media. Though highly selective organic cation exchange resins have been developed for most pollutants, they can serve as a growth medium for bacterial proliferation, impairing their long-term stability and introducing unpredictable parameters into the evolution of the system. Zeolites represent a family of inorganic cation exchangers, which naturally occur in hyper alkaline conditions and cannot serve as an electron donor or carbon source for microbial proliferation. Despite their successful application as industrial cation exchangers under near neutral conditions, their performance in hyper alkaline, saline water remains highly undocumented. Using Cs(+) as a benchmark element, this study aims to assess the long-term cation exchange performance of zeolites in concrete derived aqueous solutions. Comparison of their exchange properties in alkaline media with data obtained in near neutral solutions demonstrated that the cation exchange selectivity remains unaffected by the increased hydroxyl concentration; the cation exchange capacity did however show an unexpected increase in hyper alkaline media. PMID:25569300

  11. Absorbable microparticulate cation exchanger for immunotherapeutic delivery.

    PubMed

    Shalaby, Waleed S W; Yeh, Heidi; Woo, Edward; Corbett, Joel T; Gray, Heidi; June, Carl H; Shalaby, Shalaby W

    2004-05-15

    An absorbable microparticulate cation exchanger was synthesized as a versatile carrier for biologically active proteins. In this work, acid-terminated polyglycolide (or polyglycolic acid) microparticulates (PG-MP) were surface modified for either sustained release of cytokines or as a platform for immunomodulation. The intended goal was to achieve in situ recruitment/maturation of dendritic cells and activation of T cells for tumor immunotherapy. PG-MP were prepared with a volume weighted mean diameter of 7.02 micro (range: 2.09-14.58 micro). Accessible carboxylic acid groups were determined to be 0.3 mmol/g with a corresponding zeta potential of -21.87 mV in phosphate-buffered saline. Under low magnification, scanning electron microscopy (SEM) revealed a highly textured surface due to processing from repetitive jet milling. However, a moderately porous architecture was noted at higher magnification. Electron spectroscopy for chemical analysis was used to characterize the PG-MP surface before and after adsorption of human granulocyte-macrophage colony stimulating factor (GM-CSF). Adsorption of GM-CSF on PG-MP (PG-GMCSF) resulted in a modest increase in the surface atomic concentration of nitrogen (0.97%). Pretreating the surface with poly-L-lysine (PG/Lys-GMCSF) prior to adding GM-CSF produced a nearly threefold increase in the surface nitrogen concentration (4.20% compared to 1.47%). This manipulation not only increased loading content, but also prolonged the release of GM-CSF released from 6 days to 26 days. ESCA on the post-release PG-MP samples (PG-GMCSF and PG/Lys-GMCSF) revealed a similar residual surface nitrogen concentration (2.26% vs. 2.35%). The observation was consistent with irreversibly adsorbed GM-CSF. It is postulated that irreversibly bound GM-CSF is released over time as a function of microparticulate degradation. Biological activity of released GM-CSF was confirmed by the proliferation of a GM-CSF-dependent cell line (TF-1) in the presence of

  12. Modeling cation exchange using EQ3/6

    SciTech Connect

    Viani, B.; Bruton, C.; Bourcier, B.

    1992-08-01

    Geochemical modeling codes must be able to predict solid-solution and ion-exchange behavior of zeolites and smectites in order to design and assess strategies for containing and cleaning up toxic and/or radioactive wastes. Cation-exchange and solid-solution models have been implemented in the EQ3/6 geochemical modeling package and used to predict the composition of clinoptilolite under a variety of conditions. Published free energies of cation exchange on clinoptilolite at 25{degrees}C were combined with the calorimetric data for clinoptilolite to derive free energies of formation of the component end members of a solid solution in which mixing is allowed only on the exchange site. The solid-solution model and component end-member data were incorporated into EQ3/6 and its data base. An option to treat cation exchange independently of the solid-solution model was also developed and implemented in EQ3/6. This option allows the user to model mixed-phase exchangers, multisite exchangers, and systems in which the exchanger is not in overall equilibrium with the solution. Two {open_quotes}ideal{close_quotes} cation-exchange conventions [Vanselow (mole fraction) and Gapon (equivalent fraction)] are currently implemented in the code. A description of the cation-exchange models and their implementation into EQ3/6 is presented, and the relationship between the exchange formalisms and the solid-solution models is discussed. The advantages and limitations of the models and currently available thermodynamic data are addressed by comparing cation-exchange compositions of clinoptilolites with (1) published binary exchange data; (2) compositions of coexisting clinoptilolites and formation waters at Yucca Mountain; and (3) experimental sorption isotherms of Cs and Sr on zeolitized tuff.

  13. A Scale Model of Cation Exchange for Classroom Demonstration.

    ERIC Educational Resources Information Center

    Guertal, E. A.; Hattey, J. A.

    1996-01-01

    Describes a project that developed a scale model of cation exchange that can be used for a classroom demonstration. The model uses kaolinite clay, nails, plywood, and foam balls to enable students to gain a better understanding of the exchange complex of soil clays. (DDR)

  14. Selective Facet Reactivity During Cation Exchange in Cadmium Sulfide Nanorods

    SciTech Connect

    Sadtler, Bryce; Demchenko, Denis; Zheng, Haimei; Hughes, Steven; Merkle, Maxwell; Dahmen, Ulrich; Wang, Lin-Wang; Alivisatos, A. Paul

    2008-12-18

    The partial transformation of ionic nanocrystals through cation exchange has been used to synthesize nanocrystal heterostructures. We demonstrate that the selectivity for cation exchange to take place at different facets of the nanocrystal plays an important role in determining the resulting morphology of the binary heterostructure. In the case of copper I (Cu+) cation exchange in cadmium sulfide (CdS) nanorods, the reaction starts preferentially at the ends of the nanorods such that copper sulfide (Cu2S) grows inwards from either end. The resulting morphology is very different from the striped pattern obtained in our previous studies of silver I (Ag+) exchange in CdS nanorods where non-selective nucleation of silver sulfide (Ag2S) occurs. From interface formation energies calculated for several models of epitaxialconnections between CdS and Cu2S or Ag2S, we infer the relative stability of each interface during the nucleation and growth of Cu2S or Ag2S within the CdS nanorods. The epitaxial connections of Cu2S to the end facets of CdS nanorods minimize the formation energy, making these interfaces stable throughout the exchange reaction. However, as the two end facets of wurtzite CdS nanorods are crystallographically nonequivalent, asymmetric heterostructures can be produced.

  15. Cu Vacancies Boost Cation Exchange Reactions in Copper Selenide Nanocrystals

    PubMed Central

    2015-01-01

    We have investigated cation exchange reactions in copper selenide nanocrystals using two different divalent ions as guest cations (Zn2+ and Cd2+) and comparing the reactivity of close to stoichiometric (that is, Cu2Se) nanocrystals with that of nonstoichiometric (Cu2–xSe) nanocrystals, to gain insights into the mechanism of cation exchange at the nanoscale. We have found that the presence of a large density of copper vacancies significantly accelerated the exchange process at room temperature and corroborated vacancy diffusion as one of the main drivers in these reactions. Partially exchanged samples exhibited Janus-like heterostructures made of immiscible domains sharing epitaxial interfaces. No alloy or core–shell structures were observed. The role of phosphines, like tri-n-octylphosphine, in these reactions, is multifaceted: besides acting as selective solvating ligands for Cu+ ions exiting the nanoparticles during exchange, they also enable anion diffusion, by extracting an appreciable amount of selenium to the solution phase, which may further promote the exchange process. In reactions run at a higher temperature (150 °C), copper vacancies were quickly eliminated from the nanocrystals and major differences in Cu stoichiometries, as well as in reactivities, between the initial Cu2Se and Cu2–xSe samples were rapidly smoothed out. These experiments indicate that cation exchange, under the specific conditions of this work, is more efficient at room temperature than at higher temperature. PMID:26140622

  16. Chromatographic behaviors of proteins on cation-exchange column.

    PubMed

    Li, Rong; Chen, Guo-Liang; Zhao, Wen-Ming

    2004-12-01

    A weak cation-exchanger (XIDACE-WCX) has been synthesized by the indirect method. The chromatographic characteristics of the synthesized packing was studied in detail. The standard protein mixture and lysozyme from egg white were separated with the prepared chromatographic column. The chromatographic thermodynamics of proteins was studied in a wide temperature range. Thermodynamic parameters standard enthalpy change (deltaH0) and standard entropy change (deltaS0) and compensation temperature (beta) at protein denaturation were determined in the chromatographic system. By using obtained deltaS0, the conformational change of proteins was judged in the chromatographic process. The linear relationship between deltaH0 and deltaS0 can be used to identify the identity of the protein retention mechanism in the weak cation-exchange chromatography. The interaction between weak cation-exchanger and metal ions was investigated. Several metal chelate columns were prepared. The effects of introducing metal ion into the naked column on protein retention and the retention mechanism of proteins in the metal chalet affinity chromatography were discussed. PMID:15689030

  17. Cu Vacancies Boost Cation Exchange Reactions in Copper Selenide Nanocrystals.

    PubMed

    Lesnyak, Vladimir; Brescia, Rosaria; Messina, Gabriele C; Manna, Liberato

    2015-07-29

    We have investigated cation exchange reactions in copper selenide nanocrystals using two different divalent ions as guest cations (Zn(2+) and Cd(2+)) and comparing the reactivity of close to stoichiometric (that is, Cu2Se) nanocrystals with that of nonstoichiometric (Cu(2-x)Se) nanocrystals, to gain insights into the mechanism of cation exchange at the nanoscale. We have found that the presence of a large density of copper vacancies significantly accelerated the exchange process at room temperature and corroborated vacancy diffusion as one of the main drivers in these reactions. Partially exchanged samples exhibited Janus-like heterostructures made of immiscible domains sharing epitaxial interfaces. No alloy or core-shell structures were observed. The role of phosphines, like tri-n-octylphosphine, in these reactions, is multifaceted: besides acting as selective solvating ligands for Cu(+) ions exiting the nanoparticles during exchange, they also enable anion diffusion, by extracting an appreciable amount of selenium to the solution phase, which may further promote the exchange process. In reactions run at a higher temperature (150 °C), copper vacancies were quickly eliminated from the nanocrystals and major differences in Cu stoichiometries, as well as in reactivities, between the initial Cu2Se and Cu(2-x)Se samples were rapidly smoothed out. These experiments indicate that cation exchange, under the specific conditions of this work, is more efficient at room temperature than at higher temperature. PMID:26140622

  18. Spontaneous Superlattice Formation in Nanorods through PartialCation Exchange

    SciTech Connect

    Robinson, Richard D.; Sadtler, Bryce; Demchenko, Denis O.; Erdonmez, Can K.; Wang, Lin-Wang; Alivisatos, A. Paul

    2007-03-14

    Lattice mismatch strains are widely known to controlnanoscale pattern formation in heteroepitaxy, but such effects have notbeen exploited in colloidal nanocrystal growth. We demonstrate acolloidal route to synthesizing CdS-Ag2S nanorod superlattices throughpartial cation exchange. Strain induces the spontaneous formation ofperiodic structures. Ab initio calculations of the interfacial energy andmodeling of strain energies show that these forces drive theself-organization. The nanorod superlattices exhibit high stabilityagainst ripening and phase mixing. These materials are tunablenear-infrared emitters with potential applications as nanometer-scaleoptoelectronic devices.

  19. CATIONIC EXCHANGE PROCESS FOR THE SEPARATION OF RARE EARTHS

    DOEpatents

    Choppin, G.R.; Thompson, S.G.; Harvey, B.G.

    1960-02-16

    A process for separating mixtures of elements in the lanthanum and actinium series of the periodic table is described. The mixture of elements is dissolved in 0.05 M HCI, wherein the elements exist as tripositive ions. The resulting solution is then transferred to a column of cationic exchange resin and the column eluted with 0.1 to 0.6 M aqueous ammonium alpha hydroxy isobutyrate solution of pH 3.8 to 5.0. The use of ammonium alpha hydroxy isobutyrate as an eluting agent results in sharper and more rapid separations than previously obtainable with eluants such as citric, tartaric, glycolic, and lactic acids.

  20. Alloyed Copper Chalcogenide Nanoplatelets via Partial Cation Exchange Reactions

    PubMed Central

    2014-01-01

    We report the synthesis of alloyed quaternary and quinary nanocrystals based on copper chalcogenides, namely, copper zinc selenide–sulfide (CZSeS), copper tin selenide–sulfide (CTSeS), and copper zinc tin selenide–sulfide (CZTSeS) nanoplatelets (NPLs) (∼20 nm wide) with tunable chemical composition. Our synthesis scheme consisted of two facile steps: i.e., the preparation of copper selenide–sulfide (Cu2–xSeyS1–y) platelet shaped nanocrystals via the colloidal route, followed by an in situ cation exchange reaction. During the latter step, the cation exchange proceeded through a partial replacement of copper ions by zinc or/and tin cations, yielding homogeneously alloyed nanocrystals with platelet shape. Overall, the chemical composition of the alloyed nanocrystals can easily be controlled by the amount of precursors that contain cations of interest (e.g., Zn, Sn) to be incorporated/alloyed. We have also optimized the reaction conditions that allow a complete preservation of the size, morphology, and crystal structure as that of the starting Cu2–xSeyS1–y NPLs. The alloyed NPLs were characterized by optical spectroscopy (UV–vis–NIR) and cyclic voltammetry (CV), which demonstrated tunability of their light absorption characteristics as well as their electrochemical band gaps. PMID:25050455

  1. Monoclonal antibody capture and viral clearance by cation exchange chromatography.

    PubMed

    Miesegaes, G R; Lute, S; Strauss, D M; Read, E K; Venkiteshwaran, A; Kreuzman, A; Shah, R; Shamlou, P; Chen, D; Brorson, K

    2012-08-01

    Traditionally, post-production culture harvest capture of therapeutic monoclonal antibodies (mAbs) is performed using Protein A chromatography. We investigated the efficiency and robustness of cation exchange chromatography (CEX) in an effort to evaluate alternative capture methodologies. Up to five commercially available CEX resins were systematically evaluated using an experimentally optimized buffer platform and a design-of-experiment (DoE) approach for their ability to (a) capture a model mAb with a neutral isoelectric point, (b) clear three model viruses (porcine parvovirus, CHO type-C particles, and a bacteriophage). This approach identified a narrow operating space where yield, purity, and viral clearance were optimal under a CEX capture platform, and revealed trends between viral clearance of PPV and product purity (but not yield). Our results suggest that after unit operation optimization, CEX can serve as a suitable capture step. PMID:22488719

  2. Separation of certain carboxylic acids utilizing cation exchange membranes

    DOEpatents

    Chum, Helena L.; Sopher, David W.

    1984-01-01

    A method of substantially separating monofunctional lower carboxylic acids from a liquid mixture containing the acids wherein the pH of the mixture is adjusted to a value in the range of from about 1 to about 5 to form protonated acids. The mixture is heated to an elevated temperature not greater than about 100.degree. C. and brought in contact with one side of a perfluorinated cation exchange membrane having sulfonate or carboxylate groups or mixtures thereof with the mixture containing the protonated acids. A pressure gradient can be established across the membrane with the mixture being under higher pressure, so that protonated monofunctional lower carboxylic acids pass through the membrane at a substantially faster rate than the remainder of the mixture thereby substantially separating the acids from the mixture.

  3. Separation of certain carboxylic acids utilizing cation exchange membranes

    DOEpatents

    Chum, H.L.; Sopher, D.W.

    1983-05-09

    A method of substantially separating monofunctional lower carboxylic acids from a liquid mixture containing the acids wherein the pH of the mixture is adjusted to a value in the range of from about 1 to about 5 to form protonated acids. The mixture is heated to an elevated temperature not greater than about 100/sup 0/C and brought in contact with one side of a perfluorinated cation exchange membrane having sulfonate or carboxylate groups or mixtures thereof with the mixture containing the protonated acids. A pressure gradient can be established across the membrane with the mixture being under higher pressure, so that protonated monofunctional lower carboxylic acids pass through the membrane at a substantially faster rate than the remainder of the mixture thereby substantially separating the acids from the mixture.

  4. The kinetics of cation exchange of amorphized terskite

    NASA Astrophysics Data System (ADS)

    Chukanov, N. V.; Kazakov, A. I.; Pekov, I. V.; Grigor'eva, A. A.

    2010-12-01

    The kinetics of cation exchange between natural amorphized microporous zirconosilicate terskite Na4ZrSi6O15(OH)2 · H2O and aqueous solutions of cesium fluoride was studied calorimetrically under isothermal conditions, in the temperature range of 27.5 to 55.2°C, at CsF concentrations of 0.6-2.2 mol/l. The rate of the process was described by the first-order kinetic equation with the rate constant k, h-1 = 3.1 × 103 C {CsF/0.92} exp(-(21 ± 8) × 103/ RT). Upon replacing Na+ with Cs+, the first-order equilibrium was observed to shift abruptly toward the Cs-substituted sorbent form, where Cs2O content after saturation was 25.5-29.1 wt %. The average heat of ion exchange Q 0 over the temperature range 27.5-32.4°C was shown to be ˜3.4 kJ per 1 mol of Na+ ions. We conclude that sorbents based on A-terskite are of practical interest for the processes of extracting 137Cs isotope from water.

  5. Iridium containing honeycomb Delafossites by topotactic cation exchange.

    PubMed

    Roudebush, John H; Ross, K A; Cava, R J

    2016-06-01

    We report the structure and magnetic properties of two new iridium-based honeycomb Delafossite compounds, Cu3NaIr2O6 and Cu3LiIr2O6, formed by a topotactic cation exchange reaction. The starting materials Na2IrO3 and Li2IrO3, which are based on layers of IrO6 octahedra in a honeycomb lattice separated by layers of alkali ions, are transformed to the title compounds by a topotactic exchange reaction through heating with CuCl below 450 °C; higher temperature reactions cause decomposition. The new compounds display dramatically different magnetic behavior from their parent compounds - Cu3NaIr2O6 has a ferromagnetic like magnetic transition at 10 K, while Cu3LiIr2O6 retains the antiferromagnetic transition temperature of its parent compound but displays significantly stronger dominance of antiferromagnetic coupling between spins. These results reveal that a surprising difference in the magnetic interactions between the magnetic Ir ions has been induced by a change in the non-magnetic interlayer species. A combination of neutron and X-ray powder diffraction is used for the structure refinement of Cu3NaIr2O6 and both compounds are compared to their parent materials. PMID:27147423

  6. Using satellite data for soil cation exchange capacity studies

    NASA Astrophysics Data System (ADS)

    Ghaemi, M.; Astaraei, A. R.; Sanaeinejad, S. H.; Zare, H.

    2013-12-01

    This study was planned to examine the use of LandSat ETM+ images to develop a model for monitoring spatial variability of soil cation exchange capacity in a semi-arid area of Neyshaboor. 300 field data were collected from specific GPS registered points, 277 of which were error free, to be analysed in the soil laboratory.The statistical analysis showed that therewas a small R-Squared value, 0.17, when we used the whole data set. Visual interpretation of the graphs showed a trend among some of the data in the data set. Forty points were filtered based on the trends, and the statistical analysis was repeated for those data. It was discovered that the 40 series were more or less in the same environmental conditions; most of them were located in disturbed soils or abandoned lands with sparse vegetation cover. The soil was classified into high and medium salinity, with variable carbon (1.0 to 1.6%), heavy textured and with high silt and clay. Finally it was concluded that two different models could be fitted in the data based on their spatial dependency. The current models are able to explain spatial variability in almost 45 to 65% of the cases.

  7. Cation exchange pretreatment studies for high recovery - Yuma desalting plant

    SciTech Connect

    Kaakinen, J.W.; Laverty, P.E.

    1983-10-01

    The main purpose of the High Recovery Test Program was to obtain feasibility design data for cation exchange softening to allow a greater fractional recovery of desalted product water at the YDP(Yuma Desalting Plant). Compared to the original YDP design with 70-percent desalting recovery, additional removal of calcium in the desalting feed would allow recoveries over 90 percent. Pilot plant equipment to test this process was operated at the YDTF(Yuma Desalting Test Facility) and consisted of an IX unit and an electrodialyzer to supply reject-brine regenerant for the IX experiments. Gypsum scale buildup in the resin bed could be avoided by regeneration with a high upward flow rate causing a fluidized bed. Reuse of regenerant was also beneficial. Results show that the ion exchange high recovery pretreatment process is highly feasible, and that it is technically possible to achieve high recovery in the YDP. Numerous recommendations for a plant design are given and future studies are noted.

  8. Determination of the cation-exchange capacity of muscovite mica

    SciTech Connect

    Osman, M.A.; Suter, U.W.

    2000-04-01

    High cation-exchange capacity (CEC) muscovite mica with a homoionic surface was prepared by replacing the Li{sup +} surface ions of partially delaminated Li-mica with K{sup +}. The CEC of this K-mica was determined by exchanging its surface cations with Cs{sup +}, NH{sub 4}{sup +}, methylene blue (MB{sup +}), and copper triethylenetetramine [Cu(trien){sup 2+}]. The kinetics of these exchange reactions were studied and showed large differences depending on their relative affinities to mica. The NH{sub 4}{sup +}/K{sup +} exchange was slow, while the Cs{sup +} and Cu(trien){sup 2+}/K{sup +} exchange was fast. The MB{sup +}/K{sup +} exchange was quite slow and was not completed even after 99 h. Insufficient reaction time is one of the main reasons for the contradictory results reported in the literature for the CEC of aluminosilicates obtained by different methods. The CEC of mica can be photometrically measured by exchanging its surface cations with Cu(trien){sup 2+}.

  9. Revealing controllable nanowire transformation through cationic exchange for RRAM application.

    PubMed

    Huang, Chun-Wei; Chen, Jui-Yuan; Chiu, Chung-Hua; Wu, Wen-Wei

    2014-05-14

    One dimensional metal oxide nanostructures have attracted much attention owing to their fascinating functional properties. Among them, piezoelectricity and photocatalysts along with their related materials have stirred significant interests and widespread studies in recent years. In this work, we successfully transformed piezoelectric ZnO into photocatalytic TiO2 and formed TiO2/ZnO axial heterostructure nanowires with flat interfaces by solid to solid cationic exchange reactions in high vacuum (approximately 10(-8) Torr) transmission electron microscope (TEM). Kinetic behavior of the single crystalline TiO2 was systematically analyzed. The nanoscale growth rate of TiO2 has been measured using in situ TEM videos. On the basis of the rate, we can control the dimensions of the axial-nanoheterostructure. In addition, the unique Pt/ ZnO / TiO2/ ZnO /Pt heterostructures with complementary resistive switching (CRS) characteristics were designed to solve the important issue of sneak-peak current. The resistive switching behavior was attributed to the migration of oxygen and TiO2 layer served as reservoir, which was confirmed by energy dispersive spectrometry (EDS) analysis. This study not only supplied a distinct method to explore the transformation mechanisms but also exhibited the potential application of ZnO/TiO2 heterostructure in nanoscale crossbar array resistive random-access memory (RRAM). PMID:24742102

  10. Asphaltenes-based polymer nano-composites

    DOEpatents

    Bowen, III, Daniel E

    2013-12-17

    Inventive composite materials are provided. The composite is preferably a nano-composite, and comprises an asphaltene, or a mixture of asphaltenes, blended with a polymer. The polymer can be any polymer in need of altered properties, including those selected from the group consisting of epoxies, acrylics, urethanes, silicones, cyanoacrylates, vulcanized rubber, phenol-formaldehyde, melamine-formaldehyde, urea-formaldehyde, imides, esters, cyanate esters, allyl resins.

  11. Determining the cation exchange capacity of montmorillonite by simultaneous thermal analysis method

    NASA Astrophysics Data System (ADS)

    Boeva, N. M.; Bocharnikova, Yu. I.; Belousov, P. E.; Zhigarev, V. V.

    2016-08-01

    A way of determining the cation exchange capacity of montmorillonite by simultaneous thermal analysis is developed using as an example the bentonites of the 10th Khutor deposit (Republic of Khakassia) and the Vodopadnyi area (Sakhalin Island). A correlation is established between the cation exchange capacity of smectite and its weight loss upon heating in the range of dehydration; the enthalpy of dehydration of montmorillonite; and the weight loss and the enthalpy of thermal dissociation of ethylene glycol contained in the interlayer space of the mineral's crystal structure. These data open up new possibilities for determining the cation exchange capacity of montmorillonite, the most important technological indicator of the natural clay nanomineral.

  12. Black Carbon Increases Cation Exchange Capcity in Soils

    SciTech Connect

    Liang,B.; Lehmann, J.; Solomon, D.; Kinyangi, J.; Grossman, J.; ONeill, B.; Skjemstad, J.; Thies, J.; Luizao, F.; et al.

    2006-01-01

    Black Carbon (BC) may significantly affect nutrient retention and play a key role in a wide range of biogeochemical processes in soils, especially for nutrient cycling. Anthrosols from the Brazilian Amazon (ages between 600 and 8700 yr BP) with high contents of biomass-derived BC had greater potential cation exchange capacity (CEC measured at pH 7) per unit organic C than adjacent soils with low BC contents. Synchrotron-based near edge X-ray absorption fine structure (NEXAFS) spectroscopy coupled with scanning transmission X-ray microscopy (STXM) techniques explained the source of the higher surface charge of BC compared with non-BC by mapping cross-sectional areas of BC particles with diameters of 10 to 50 {micro}m for C forms. The largest cross-sectional areas consisted of highly aromatic or only slightly oxidized organic C most likely originating from the BC itself with a characteristic peak at 286.1 eV, which could not be found in humic substance extracts, bacteria or fungi. Oxidation significantly increased from the core of BC particles to their surfaces as shown by the ratio of carboxyl-C/aromatic-C. Spotted and non-continuous distribution patterns of highly oxidized C functional groups with distinctly different chemical signatures on BC particle surfaces (peak shift at 286.1 eV to a higher energy of 286.7 eV) indicated that non-BC may be adsorbed on the surfaces of BC particles creating highly oxidized surface. As a consequence of both oxidation of the BC particles themselves and adsorption of organic matter to BC surfaces, the charge density (potential CEC per unit surface area) was greater in BC-rich Anthrosols than adjacent soils. Additionally, a high specific surface area was attributable to the presence of BC, which may contribute to the high CEC found in soils that are rich in BC.

  13. Several textural properties of compacted and cation-exchanged bentonite

    NASA Astrophysics Data System (ADS)

    Montes-Hernandez, G.; Duplay, J.; Géraud, Y.; Martinez, L.

    2006-08-01

    One of the principal applications for bentonite is in drilling muds. Moreover it is widely used as a suspending and stabilizing agent, and as an adsorbent or clarifying agent, in many industries. Recently the bentonites have been proposed as engineered barriers for radioactive waste repository because these materials are supposed to build up a better impermeable zone around wastes by swelling. For these reasons, a textural characterization of bentonites in the laboratory is very important. The aim in this study was to estimate several textural properties of compacted and cation-exchanged bentonite by using Hg-porosimetry, N2-adsorption, water vapour adsorption, scanning electron microscopy (SEM) observations and environmental scanning electron microscopy-digital images analysis measurements. For that, bulk samples were mechanically compressed at atmospheric conditions by using a uniaxial system at four different pressures (21, 35, 49, and 63 MPa) in order to obtain four physical densities. On the other hand, the bulk samples of bentonite were treated separately with four concentrated solutions (1N concentration) of sodium, potassium, magnesium and calcium chlorides in order to obtain a homoionic interlayer cation in the clay phase. The results showed that the macro-porosity (porous size>50 nm) and eventually the mesoporosity (porous size 2 50 nm) are affected by the uniaxial compaction. In this case, a transformation of the shape of the macro-pores network from tube to crack was observed. On the other hand, the swelling potential and water content are governed by the relative humidity and by the nature of interlayer cation.

  14. Mechanical Properties of Polymer Nano-composites

    NASA Astrophysics Data System (ADS)

    Srivastava, Iti

    Thermoset polymer composites are increasingly important in high-performance engineering industries due to their light-weight and high specific strength, finding cutting-edge applications such as aircraft fuselage material and automobile parts. Epoxy is the most widely employed thermoset polymer, but is brittle due to extensive cross-linking and notch sensitivity, necessitating mechanical property studies especially fracture toughness and fatigue resistance, to ameliorate the low crack resistance. Towards this end, various nano and micro fillers have been used with epoxy to form composite materials. Particularly for nano-fillers, the 1-100 nm scale dimensions lead to fascinating mechanical properties, oftentimes proving superior to the epoxy matrix. The chemical nature, topology, mechanical properties and geometry of the nano-fillers have a profound influence on nano-composite behavior and hence are studied in the context of enhancing properties and understanding reinforcement mechanisms in polymer matrix nano-composites. Using carbon nanotubes (CNTs) as polymer filler, uniquely results in both increased stiffness as well as toughness, leading to extensive research on their applications. Though CNTs-polymer nano-composites offer better mechanical properties, at high stress amplitude their fatigue resistance is lost. In this work covalent functionalization of CNTs has been found to have a profound impact on mechanical properties of the CNT-epoxy nano-composite. Amine treated CNTs were found to give rise to effective fatigue resistance throughout the whole range of stress intensity factor, in addition to significantly enhancing fracture toughness, ductility, Young's modulus and average hardness of the nano-composite by factors of 57%, 60%, 30% and 45% respectively over the matrix as a result of diminished localized cross-linking. Graphene, a one-atom-thick sheet of atoms is a carbon allotrope, which has garnered significant attention of the scientific community and is

  15. Tuning the Magnetic Properties of Metal Oxide Nanocrystal Heterostructures by Cation Exchange

    PubMed Central

    2013-01-01

    For three types of colloidal magnetic nanocrystals, we demonstrate that postsynthetic cation exchange enables tuning of the nanocrystal’s magnetic properties and achieving characteristics not obtainable by conventional synthetic routes. While the cation exchange procedure, performed in solution phase approach, was restricted so far to chalcogenide based semiconductor nanocrystals, here ferrite-based nanocrystals were subjected to a Fe2+ to Co2+ cation exchange procedure. This allows tracing of the compositional modifications by systematic and detailed magnetic characterization. In homogeneous magnetite nanocrystals and in gold/magnetite core shell nanocrystals the cation exchange increases the coercivity field, the remanence magnetization, as well as the superparamagnetic blocking temperature. For core/shell nanoheterostructures a selective doping of either the shell or predominantly of the core with Co2+ is demonstrated. By applying the cation exchange to FeO/CoFe2O4 core/shell nanocrystals the Neél temperature of the core material is increased and exchange-bias effects are enhanced so that vertical shifts of the hysteresis loops are obtained which are superior to those in any other system. PMID:23362940

  16. Atomistic understanding of cation exchange in PbS nanocrystals using simulations with pseudoligands

    NASA Astrophysics Data System (ADS)

    Fan, Zhaochuan; Lin, Li-Chiang; Buijs, Wim; Vlugt, Thijs J. H.; van Huis, Marijn A.

    2016-05-01

    Cation exchange is a powerful tool for the synthesis of nanostructures such as core-shell nanocrystals, however, the underlying mechanism is poorly understood. Interactions of cations with ligands and solvent molecules are systematically ignored in simulations. Here, we introduce the concept of pseudoligands to incorporate cation-ligand-solvent interactions in molecular dynamics. This leads to excellent agreement with experimental data on cation exchange of PbS nanocrystals, whereby Pb ions are partially replaced by Cd ions from solution. The temperature and the ligand-type control the exchange rate and equilibrium composition of cations in the nanocrystal. Our simulations reveal that Pb ions are kicked out by exchanged Cd interstitials and migrate through interstitial sites, aided by local relaxations at core-shell interfaces and point defects. We also predict that high-pressure conditions facilitate strongly enhanced cation exchange reactions at elevated temperatures. Our approach is easily extendable to other semiconductor compounds and to other families of nanocrystals.

  17. Glutathione-based zwitterionic stationary phase for hydrophilic interaction/cation-exchange mixed-mode chromatography.

    PubMed

    Shen, Aijin; Li, Xiuling; Dong, Xuefang; Wei, Jie; Guo, Zhimou; Liang, Xinmiao

    2013-11-01

    As a naturally hydrophilic peptide, glutathione was facilely immobilized onto silica surface to obtain a novel hydrophilic interaction/cation-exchange mixed-mode chromatographic stationary phase (Click TE-GSH) via copper-free "thiol-ene" click chemistry. The resulting material was characterized by solid state (13)C/CP MAS NMR and elemental analysis. The measurement of ζ-potential indicated the cation-exchange characteristics and adjustable surface charge density of Click TE-GSH material. The influence of acetonitrile content and pH value on the retention of ionic compounds was investigated for understanding the chromatographic behaviors. The results demonstrated that Click TE-GSH column could provide both hydrophilic and cation-exchange interaction. Taking advantage of the good hydrophilicity and inherent cation-exchange characteristics of Click TE-GSH material, the resolution of neutral fructosan with high degree of polymerization (DP), basic chitooligosaccharides and strongly acidic carrageenan oligosaccharides was successfully realized in hydrophilic interaction chromatography (HILIC), hydrophilic interaction/cation-exchange mixed-mode chromatography (HILIC/CEX), cation-exchange chromatography (CEX) and electrostatic repulsion/hydrophilic interaction chromatography (ERLIC). On the other hand, the separation of standard peptides varying in hydrophobicity/hydrophilicity and charge was achieved in both CEX and HILIC/CEX mode with high efficiency and distinct selectivity. To further demonstrate the versatility and applicability of Click TE-GSH stationary phase, the separation of a human serum albumin (HSA) tryptic digest was performed in HILIC/CEX mode. Peptides were adequately resolved and up to 86 HSA peptides were identified with sequence coverage of 85%. The results indicated the good potential of Click TE-GSH material in glycomics and proteomics. PMID:24075460

  18. Cation Exchange Reactions for Improved Quality and Diversity of Semiconductor Nanocrystals

    NASA Astrophysics Data System (ADS)

    Beberwyck, Brandon James

    Observing the size and shape dependent physical properties of semiconductor nanocrystals requires synthetic methods capable of not only composition and crystalline phase control but also molecular scale uniformity for a particle consisting of tens to hundreds of thousands of atoms. The desire for synthetic methods that produce uniform nanocrystals of complex morphologies continues to increase as nanocrystals find roles in commercial applications, such as biolabeling and display technologies, that are simultaneously restricting material compositions. With these constraints, new synthetic strategies that decouple the nanocrystal's chemical composition from its morphology are necessary. This dissertation explores the cation exchange reaction of colloidal semiconductor nanocrystals, a template-based chemical transformation that enables the interconversion of nanocrystals between a variety of compositions while maintaining their size dispersity and morphology. Chapter 1 provides an introduction to the versatility of this replacement reaction as a synthetic method for semiconductor nanocrystals. An overview of the fundamentals of the cation exchange reaction and the diversity of products that are achievable is presented. Chapter 2 examines the optical properties of nanocrystal heterostructures produced through cation exchange reactions. The deleterious impact of exchange on the photoluminescence is correlated to residual impurities and a simple annealing protocol is demonstrated to achieve photoluminescence yields comparable to samples produced by conventional methods. Chapter 3 investigates the extension of the cation exchange reaction beyond ionic nanocrystals. Covalent III-V nanocrystal of high crystallinity and low size dispersity are synthesized by the cation exchange of cadmium pnictide nanocrystals with group 13 ions. Lastly, Chapter 4 highlights future studies to probe cation exchange reactions in colloidal semiconductor nanocrystals and progress that needs to be

  19. NUTRIENT LEACHING FROM CONIFER NEEDLES IN RELATION TO FOLIAR APOPLAST CATION EXCHANGE CAPACITY

    EPA Science Inventory

    Limited evidence to date suggests that acidic precipitation promotes leaching of nutrient cations from conifer foliage. n order to evaluate the relative contribution of the apoplast cation exchange complex and symplast nutrient pools to the leached ions, the magnitude of potentia...

  20. Influence of pine bark particle size and pH on cation exchange capacity

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Cation exchange capacity (CEC) describes the maximum quantity of cations a soil or substrate can hold while being exchangeable with the soil solution. While CEC has been studied for peat-based substrates, relatively little work has documented factors that affect CEC of pine bark substrates. The ob...

  1. Selective separation of sodium ions from a mixture with phenylalanine by Donnan dialysis with a profiled sulfogroup cation exchange membrane

    NASA Astrophysics Data System (ADS)

    Vasil'eva, V. I.; Goleva, E. A.

    2013-11-01

    The possibility of separating ions of metal from a mixture with ampholyte (an amino acid) by Donnan dialysis with an MK-40 sulfogroup cation exchange membrane is demonstrated. Conditions ensuring the selectivity and intensity of the mass transfer of sodium ions from a mixture with bipolar phenylalanine ions into a diffusate containing hydrochloric acid through a cation exchange membrane are found.

  2. Synthesis and characterization of new electroactive polypyrrole-chondroitin sulphate A substrates.

    PubMed

    Serra Moreno, J; Panero, S; Artico, M; Filippini, P

    2008-02-01

    Novel composite polypyrrole/chondroitin-4-sulphate films with cation-exchange properties were synthesized by the electrochemical polymerization of pyrrole in the presence of chondroitin-4-sulphate (CSA) sodium salt, acting as dopant anion at neutral pH. The negatively charged biomolecule was found to be permanently entrapped in the polypyrrole (PPy) membrane which resulted, as expected, facilitated in the mass transport by mobile cationic counterions. The porous nature of the substrates was identified as the most influential factor controlling the morphology. The morphology, in turn, affects the interaction between the material surface and the tissues on a cellular level. In this work in vitro analyses of human fibroblast response to polypyrrole/chondroitin-4-sulphate films were performed to focus on the different steps of cell reactions towards defined surface properties. PMID:18155969

  3. X-ray Studies of Nano Composites

    NASA Astrophysics Data System (ADS)

    Hexemer, Alexander

    Nano composite materials are an exciting and fast expanding field. X-ray scattering has been used in order to study the structure properties relation. During the last few years the field has expanded more towards the field of thin films where there's been a dramatic increase in the use of grazing incidence small angle X-ray scattering (GISAXS). The main issue of GISAXS has been the complex analysis framework necessary for simulating and fitting. In addition, existing software has restricted the scientist in systems that can be simulated and the speed to analyze large amounts of data. Over the last few years we have worked closely with our computational research and supercomputer division to enable the use of supercomputers to simulate at scattering data. We have developed a comprehensive analysis framework to simulate and fit a wide variety of materials and morphologies. The framework is designed to supply scientists with close to real-time feedback during beam times. Therefore, HipGISAXS (High Performance GISAXS) has been developed to run simulations on massively parallel platforms such as the Oak Ridge Supercomputer Titan (OLCF). Further, with inverse modeling algorithms for fitting available in HipGISAXS, such as particle swarm optimization, it can handle a large number of parameters during the structure fitting process. In September of 2014, HipGISAXS was used in a real time demonstration that married the SAXS/WAXS beamline at the ALS with the data handling and processing capabilities at NERSC, and simulation capabilities of running at-scale simulations on Titan at OLCF. Doe Early Carrier Award, SPOT and CAMERA.

  4. Nano composite phase change materials microcapsules

    NASA Astrophysics Data System (ADS)

    Song, Qingwen

    MicroPCMs with nano composite structures (NC-MicroPCMs) have been systematically studied. NC-MicroPCMs were fabricated by the in situ polymerization and addition of silver NPs into core-shell structures. A full factorial experiment was designed, including three factors of core/shell, molar ratio of formaldehyde/melamine and NPs addition. 12 MicroPCMs samples were prepared. The encapsulated efficiency is approximately 80% to 90%. The structural/morphological features of the NC-MicroPCMs were evaluated. The size was in a range of 3.4 mu m to 4.0 mu m. The coarse appearance is attributed to NPs and NPs are distributed on the surface, within the shell and core. The NC-MicroPCMs contain new chemical components and molecular groups, due to the formation of chemical bonds after the pretreatment of NPs. Extra X-ray diffraction peaks of silver were found indicating silver nano-particles were formed into an integral structure with the core/shell structure by means of chemical bonds and physical linkages. Extra functionalities were found, including: (1) enhancement of IR radiation properties; (2) depression of super-cooling, and (3) increase of thermal stabilities. The effects of SERS (Surface Enhanced Raman Spectroscopy) arising from the silver nano-particles were observed. The Raman scattering intensity was magnified more than 100 times. These effects were also exhibited in macroscopic level in the fabric coatings as enhanced IR radiation properties were detected by the "Fabric Infrared Radiation Management Tester" (FRMT). "Degree of Crystallinity" (DOC) was measured and found the three factors have a strong influence on it. DOC is closely related to thermal stability and MicroPCMs with a higher DOC show better temperature resistance. The thermal regulating effects of the MicroPCMs coatings were studied. A "plateau regions" was detected around the temperature of phase change, showing the function of PCMs. Addition of silver nano-particles to the MicroPCMs has a positive

  5. Sequential Anion and Cation Exchange Reactions for Complete Material Transformations of Nanoparticles with Morphological Retention.

    PubMed

    Hodges, James M; Kletetschka, Karel; Fenton, Julie L; Read, Carlos G; Schaak, Raymond E

    2015-07-20

    Ion exchange reactions of colloidal nanocrystals provide access to complex products that are synthetically challenging using traditional hot-injection methods. However, such reactions typically achieve only partial material transformations by employing either cation or anion exchange processes. It is now shown that anion and cation exchange reactions can be coupled together and applied sequentially in one integrated pathway that leads to complete material transformations of nanocrystal templates. Although the product nanocrystals do not contain any of the original constituent elements, the original morphology is retained, thereby fully decoupling morphology and composition control. The sequential anion/cation exchange process was applied to pseudo-spherical CdO nanocrystals and ZnO tetrapods, producing fully transformed and shape-controlled nanocrystals of copper and silver sulfides and selenides. Furthermore, hollow core-shell tetrapod ZnS@CdS heterostructures were readily accessible. PMID:26110653

  6. Study by XPS of different conditioning processes to improve the cation exchange in clinoptilolite

    NASA Astrophysics Data System (ADS)

    Ruiz-Serrano, D.; Flores-Acosta, M.; Conde-Barajas, E.; Ramírez-Rosales, D.; Yáñez-Limón, J. M.; Ramírez-Bon, R.

    2010-09-01

    We report the X-ray photoelectron spectroscopy (XPS) analysis of natural clinoptilolite from a mine in Sonora, México. From these measurements we determined the chemical state and binding energy of the elements in the zeolite framework and of those in the extra framework sites. The analysis was done on natural clinoptilolite and on cation-exchanged clinoptilolites with Na + and NH4+ ions. Complementary analysis by several experimental techniques was performed to determine the structural, chemical composition and chemical state modifications experimented by clinoptilolite samples processed by the two types of cation exchange. The clinoptilolite samples were studied by X-ray powder diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR) to determine their structural composition, Energy Dispersive Spectroscopy (EDS) to measure the chemical composition and electronic paramagnetic resonance (EPR) spectroscopy to determine the chemical state of iron inside the natural zeolites.

  7. Aspects of the super-equivalent sorption of glycine by cation exchanger KU-2-8

    NASA Astrophysics Data System (ADS)

    Khokhlova, O. N.; Khokhlov, V. Yu.; Trunaeva, E. S.; Nechaeva, L. S.

    2016-07-01

    The structure formed in a sorbent during the super-equivalent sorption of glycine by cation exchanger KU-2-8 is optimized via quantum chemical simulation. The differential thermodynamic characteristics of ion exchange and super-equivalent sorption in the studied system are calculated using a thermodynamic approach that allows us to describe the simultaneous exchange and super-equivalent sorption of compounds by ion-exchangers.

  8. Emission spectrographic determination of barium in sea water using a cation exchange concentration procedure

    USGS Publications Warehouse

    Szabo, B. J.; Joensuu, O.

    1967-01-01

    A concentration technique employing Dowex 50W cation exchange resin is described for the determination of barium in sea water. The separated barium is precipitated as fluoride together with calcium and strontium and measured by emission spectrographic analysis. The vertical distribution of barium in sea water has been measured in the Caribbean Sea and the Atlantic Ocean. The barium content varied between 7 and 23 ??g. per liter; in two profiles, the lowest concentrations were at a depth of about 1000 meters.

  9. Log-derived cation exchange capacity of shaly sands: Application to hydrocarbon detection and drilling optimization

    NASA Astrophysics Data System (ADS)

    Ipek, Gamze

    Researchers at Louisiana State University, LSU, have introduced several petrophysical models expressing the electric properties of shaly sands. These models, to be used for hydrocarbon detection, are based on the Waxman and Smits concept of supplementing the water conductivity with a clay counterions conductivity. The LSU models also utilize the Dual Water theory, which relates each conductivity term to a particular type of water, free and bound, each occupying a specific volume of the total pore space. The main difference between these models and the other shaly sand models is that the counterion conductivity is represented by a hypothetical sodium chloride electrolyte. This study introduces a modified version of early LSU models. This modified model eliminates a questionable assumption incorporated in all previous shaly sand models. Previous models use same formation resistivity factor for all terms in the model. The proposed model considers that the electric current follows the effective porosity path in the term representing the free electrolyte and follows the clay porosity path in the term representing bound water. The differentiation between the two paths is accomplished by using two different formation factors one in the free water and another in the bound water term of the model. It also used two different cementation exponents to express formation factors in terms of porosity. The validity of the new model was checked using cation exchange capacities measured on core samples and drill cuttings. Calculated cation exchange capacities display good agreement with the measured cation exchange capacities. The water saturation calculated using the new model are more representative of hydrocarbon potential of the zones of interest. In addition, cation exchange capacity calculated using this modified model and log data acquired during drilling has shown potential for diagnosis of pending bit balling of PDC bits drilled with water based mud in overpressured shale.

  10. Atomistic understanding of cation exchange in PbS nanocrystals using simulations with pseudoligands

    PubMed Central

    Fan, Zhaochuan; Lin, Li-Chiang; Buijs, Wim; Vlugt, Thijs J. H.; van Huis, Marijn A.

    2016-01-01

    Cation exchange is a powerful tool for the synthesis of nanostructures such as core–shell nanocrystals, however, the underlying mechanism is poorly understood. Interactions of cations with ligands and solvent molecules are systematically ignored in simulations. Here, we introduce the concept of pseudoligands to incorporate cation-ligand-solvent interactions in molecular dynamics. This leads to excellent agreement with experimental data on cation exchange of PbS nanocrystals, whereby Pb ions are partially replaced by Cd ions from solution. The temperature and the ligand-type control the exchange rate and equilibrium composition of cations in the nanocrystal. Our simulations reveal that Pb ions are kicked out by exchanged Cd interstitials and migrate through interstitial sites, aided by local relaxations at core–shell interfaces and point defects. We also predict that high-pressure conditions facilitate strongly enhanced cation exchange reactions at elevated temperatures. Our approach is easily extendable to other semiconductor compounds and to other families of nanocrystals. PMID:27160371

  11. Preparation and Characterization of Cotton Textile Graft Copolymers as Cation Exchanger

    NASA Astrophysics Data System (ADS)

    Mostafa, Kh. M.

    2005-03-01

    Acrylic Acid (AA) was graft copolymerized with cotton cellulose in fabric form to prepare poly (AA)-cotton graft copolymer cation exchanger using Fe2+/BrO3- redox system in aqueous medium under a nitrogen atmosphere. The effect of Fe2+, BrO3- and monomer concentrations, pH as well as time and temperature of polymerization were studied by determining the grafting parameters gravimetrically, like Graft Yield (GY %) and Graft Reaction Efficiency (GRE %). On the other hand, the newly prepared poly (AA)-cotton graft copolymers were characterized for different heavy metals ions removal to determined their suitability as cation exchanger. On the basis of a detailed investigation of the above factors, the appropriate conditions for grafting were as follows: Fe2+, 0.005 mol L-1; BrO3-, 0.001 mol L-1; pH, 2; monomer, (50% based on weight of substrate); time, 90 min and temperature, 35°C. On the other hand, the potential value of the newly prepared poly (AA)-cotton graft copolymer to serve as cation exchanger was assessed through measurements of critical properties such as removal of different heavy metal ions from their solutions as well as durability.

  12. Impact of sediment-seawater cation exchange on Himalayan chemical weathering fluxes

    NASA Astrophysics Data System (ADS)

    Lupker, Maarten; France-Lanord, Christian; Lartiges, Bruno

    2016-08-01

    Continental-scale chemical weathering budgets are commonly assessed based on the flux of dissolved elements carried by large rivers to the oceans. However, the interaction between sediments and seawater in estuaries can lead to additional cation exchange fluxes that have been very poorly constrained so far. We constrained the magnitude of cation exchange fluxes from the Ganga-Brahmaputra river system based on cation exchange capacity (CEC) measurements of riverine sediments. CEC values of sediments are variable throughout the river water column as a result of hydrological sorting of minerals with depth that control grain sizes and surface area. The average CEC of the integrated sediment load of the Ganga-Brahmaputra is estimated ca. 6.5 meq 100 g-1. The cationic charge of sediments in the river is dominated by bivalent ions Ca2+ (76 %) and Mg2+ (16 %) followed by monovalent K+ (6 %) and Na+ (2 %), and the relative proportion of these ions is constant among all samples and both rivers. Assuming a total exchange of exchangeable Ca2+ for marine Na+ yields a maximal additional Ca2+ flux of 28 × 109 mol yr-1 of calcium to the ocean, which represents an increase of ca. 6 % of the actual river dissolved Ca2+ flux. In the more likely event that only a fraction of the adsorbed riverine Ca2+ is exchanged, not only for marine Na+ but also Mg2+ and K+, estuarine cation exchange for the Ganga-Brahmaputra is responsible for an additional Ca2+ flux of 23 × 109 mol yr-1, while ca. 27 × 109 mol yr-1 of Na+, 8 × 109 mol yr-1 of Mg2+ and 4 × 109 mol yr-1 of K+ are re-absorbed in the estuaries. This represents an additional riverine Ca2+ flux to the ocean of 5 % compared to the measured dissolved flux. About 15 % of the dissolved Na+ flux, 8 % of the dissolved K+ flux and 4 % of the Mg2+ are reabsorbed by the sediments in the estuaries. The impact of estuarine sediment-seawater cation exchange appears to be limited when evaluated in the context of the long-term carbon cycle and

  13. Effect of cation exchange on surfactant-enhanced solubilization of trichloroethene

    NASA Astrophysics Data System (ADS)

    Field, J. A.; Sawyer, T. E.; Schroth, M. H.; Humphrey, M. D.; Istok, J. D.

    2000-11-01

    The objective of this study was to develop the single-well push-pull test as a diagnostic tool for assessing the potential for cation exchange to adversely affect the phase behavior of sodium dihexyl sulfosuccinate surfactant (Aerosol MA 80-I) and its solubilization of trichloroethene (TCE) in the subsurface. Laboratory push-pull tests were conducted on a model natural aquifer sediment collected from a TCE-contaminated field site and a test solution consisting of 36,800 mg/l (3.7 wt.%) sulfosuccinate, 100,000 mg/l (10 wt.%) isopropanol, and 3200 mg/l (0.32 wt.%) KBr. Laboratory experiments were designed to simulate conditions occurring during single-well, "push-pull" tests. In batch experiments conducted in the presence of excess TCE, the test solution gave a Winsor Type I system with an enhanced aqueous TCE solubility of 26,700 mg/l and a solution density of 1.000 g/cm 3. The sulfosuccinate surfactant was transported conservatively in sediment packs containing no TCE. However, increasing concentrations of Ca 2+ and Mg 2+ resulting from cation exchange caused the TCE solubilization potential of the injected surfactant to exceed values predicted from the solubilization isotherm. Sulfosuccinate surfactant transport was strongly retarded in sediment packs containing 5 vol.% residual TCE because cation exchange resulted in the formation of a Winsor Type II system, which resulted in the partitioning of the sulfosuccinate surfactant into the residual TCE phase. Conservative sulfosuccinate transport was observed in a separate sediment pack containing 5 vol.% residual TCE when a 130 meq/l Na + pre-flush was used to reduce quantities of Ca 2+ and Mg 2+ in the sediment pack prior to sulfosuccinate injection. The results of this study emphasize the importance of cation exchange on the performance of surfactant-enhanced TCE solubilization and demonstrate the utility of the push-pull test for predicting the potentially deleterious effects of cation exchange on surfactant phase

  14. Sorption of REE and TPE from HNO{sub 3} solutions on strong-acid sulfonated cation exchanger KU-2

    SciTech Connect

    Chuveleva, E.A.; Kharitonov, O.V.; Firsova, L.A.

    1995-05-01

    Sorption of rare earths (REE) on the strong-acid sulfonated cation exchanger KU-2 is studied as a function of the solution acidity (0.1-2.0 M HNO{sub 3}) and REE concentration. In concentrated nitrate solutions where M(NO{sub 3}){sub 2}{sup +} and M(NO{sub 3}){sub 2}{sup +} can form and be sorbed by the cation exchanger, the capacity of the exchanger seems to increase by 20%.

  15. Nano-Composite Material Development for 3-D Printers

    SciTech Connect

    Satches, Michael Randolph

    2015-10-14

    The objectives of the project was to create a graphene reinforced polymer nano-composite viable in a commercial 3-D printer; study the effects of ultra-high loading of graphene in polymer matrices; and determine the functional upper limit of graphene loading.

  16. Cation exchange in a glacial till drumlin at a road salt storage facility.

    PubMed

    Ostendorf, David W; Xing, Baoshan; Kallergis, Niki

    2009-05-12

    We use laboratory and field data to calibrate existing geochemical and transport models of cation exchange induced by contamination of an unconfined aquifer at a road salt storage facility built upon a glacial till drumlin in eastern Massachusetts. A Gaines and Thomas selectivity coefficient K models the equilibrium sodium and divalent cation distribution in the groundwater and solid matrix, while an existing method of characteristics model describes the advective transport of total dissolved cations and sorbed sodium. Laboratory isotherms of split spoon soil samples from the drumlin calibrate K with an average value of 0.0048 (L/g)(1/2) for a measured cation exchange capacity of 0.057 meq/g dry soil. Ten years of monitoring well data document groundwater flow and the advection of conservative chloride due to outdoor storage and handling of road salt at the site. The monitoring well cation data and retarded transport model offer an independent K calibration of 0.0040 to 0.0047 (L/g)(1/2): the consistency of the field and laboratory selectivity coefficient calibrations endorse this application of the Gaines and Thomas and method of characteristics models. The advancing deicing agent plume releases divalent cations from the till into the groundwater, so that monitoring well samples do not reflect the chemical composition of the road salt. In this regard, dissolved divalent cation milliequivalent concentrations are as high as 80% of the total dissolved cationic concentrations in the salt contaminated monitoring well samples, far greater than their 2.5% level in the road salt stored at the site. Cation exchange can thus obscure attempts to hindcast stored road salt sodium water table concentration from monitoring well sample stoichiometry, or to predict sodium impacts on groundwater or receiving stream quality downgradient of the well. PMID:19272668

  17. Cation exchange in a glacial till drumlin at a road salt storage facility

    NASA Astrophysics Data System (ADS)

    Ostendorf, David W.; Xing, Baoshan; Kallergis, Niki

    2009-05-01

    We use laboratory and field data to calibrate existing geochemical and transport models of cation exchange induced by contamination of an unconfined aquifer at a road salt storage facility built upon a glacial till drumlin in eastern Massachusetts. A Gaines and Thomas selectivity coefficient K models the equilibrium sodium and divalent cation distribution in the groundwater and solid matrix, while an existing method of characteristics model describes the advective transport of total dissolved cations and sorbed sodium. Laboratory isotherms of split spoon soil samples from the drumlin calibrate K with an average value of 0.0048 (L/g) 1/2 for a measured cation exchange capacity of 0.057 meq/g dry soil. Ten years of monitoring well data document groundwater flow and the advection of conservative chloride due to outdoor storage and handling of road salt at the site. The monitoring well cation data and retarded transport model offer an independent K calibration of 0.0040 to 0.0047 (L/g) 1/2: the consistency of the field and laboratory selectivity coefficient calibrations endorse this application of the Gaines and Thomas and method of characteristics models. The advancing deicing agent plume releases divalent cations from the till into the groundwater, so that monitoring well samples do not reflect the chemical composition of the road salt. In this regard, dissolved divalent cation milliequivalent concentrations are as high as 80% of the total dissolved cationic concentrations in the salt contaminated monitoring well samples, far greater than their 2.5% level in the road salt stored at the site. Cation exchange can thus obscure attempts to hindcast stored road salt sodium water table concentration from monitoring well sample stoichiometry, or to predict sodium impacts on groundwater or receiving stream quality downgradient of the well.

  18. Comparison of commercial cation exchange media for performing marine Toxicity Identification Evaluations (TIEs)

    SciTech Connect

    Charles, J.B.; Burgess, R.M.; Kuhn, A.; Ho, K.T.

    1995-12-31

    In the environment, adverse effects of metals resulting from anthropogenic activity can be manifested as effluent, receiving water, and sediment toxicity to aquatic organisms. In TIEs, the chelator EDTA is commonly used to discriminate metal toxicity from other possible sources of toxicity present in an environmental sample. EDTA is extremely effective at reducing the aqueous bioavailability of toxic divalent transition metals (e.g., Cd, Cu, Ni, Pb, Zn) but, unlike C{sub 18} solid phase extraction (SPE), EDTA does not allow for retrieval of toxicity or toxicants for further identification. In this presentation, the authors report the results of comparisons of five commercially available cation exchange media for use in TIEs. Cation exchange media included three pre-packed SPE columns (Alltech, Supelco, Waters) and two loose packing materials evaluated with both metal spiked seawater and deionized water. Preliminary comparisons demonstrated that Alltech and Supelco SPE columns functioned most effectively. Blank toxicity to two marine species was not observed. Extensive studies of Alltech and Supelco columns using seawater spiked with a range of metal concentrations (e.g., 600 to 10 {micro}g/L) illustrated good precision and quality. both columns removed, on average, {ge} 90% of five metals from seawater. Furthermore, when eluted with small volumes of acid, {ge} 85% of original metal levels were recovered. Evaluations performed with a metal plating industry effluent demonstrated effective removal and subsequent elution of several toxic metals. This study shows the utility of commercial cation exchange columns for removing metals from seawater, and freshwater, for TIE applications.

  19. Effect of pH on protein adsorption capacity of strong cation exchangers with grafted layer.

    PubMed

    Wrzosek, Katarzyna; Polakovič, Milan

    2011-09-28

    The effect of pH on the static adsorption capacity of immunoglobulin G, human serum albumin, and equine myoglobin was investigated for a set of five strong cation exchangers with the grafted tentacle layer having a different ligand density. A sharp maximum of adsorption capacity with pH was observed for adsorbents with a high ligand density. The results were elucidated using the protein structure and calculations of pK(a) of ionizable groups of surface basic residues. Inverse size-exclusion experiments were carried out to understand the relation between the adsorption capacity and pore accessibility of the investigated proteins. PMID:21855072

  20. Improved Proteome and Phosphoproteome Analysis on a Cation Exchanger by a Combined Acid and Salt Gradient.

    PubMed

    Adachi, Jun; Hashiguchi, Kazunari; Nagano, Maiko; Sato, Misako; Sato, Ayako; Fukamizu, Kazuna; Ishihama, Yasushi; Tomonaga, Takeshi

    2016-08-16

    Currently used elution methods for strong cation exchange (SCX) chromatography are based on two principles: salt and pH gradient. In this paper, we report the first observation of peptide elution by acid gradient. The degree of peptide separation using C18-SCX StageTip was greatly improved by our acid and salt-based elution method compared with a salt-based elution method. This development enabled us to identify over 22 000 phosphopeptides from 2 mg of protein without labor-intensive sample preparation. Our method is simple, robust, scalable, and low-cost and can be easily implemented without any special equipment or techniques. PMID:27436111

  1. In vitro adsorption removal of paraquat by activated carbon and cation exchange resin

    SciTech Connect

    Kitakouji, M.; Miyoshi, T.; Tanada, M.S.; Nakamura, T. )

    1989-06-01

    With the modernization of agriculture, environmental pollution and accidental poisoning by agricultural chemicals have become a great social problem. With the remarkable increase in the amount of paraquat used, the number of deaths by swallowing of paraquat has also increased in recent years. Presently, an effective antidote and treatment for paraquat poisoning is not available. For primary treatment, administration of an adsorbent is done at the same time as gastrointestinal lavage. As an adsorbent for paraquat poisoning, the efficacy of activated carbon, Fuller's Earth, bentonite, and a cation exchange resin have been reported. In this work, the authors discuss the adsorption characteristics of paraquat in artificial gastric juice and normal saline solution.

  2. Cation-exchange chromatography of peptides on poly(2-sulfoethyl aspartamide)-silica.

    PubMed

    Alpert, A J; Andrews, P C

    1988-06-29

    A strong cation-exchange material, poly(2-sulfoethyl aspartamide)-silica (PolySULFOETHYL Aspartamide) was developed for purification and analysis of peptides by high-performance liquid chromatography. All peptides examined were retained at pH 3, even when the amino terminus was the only basic group. Peptides were eluted in order of increasing number of basic residues with a salt gradient. Capacity was high, as was selectivity and column efficiency. This new column material displays modest mixed-mode effects, allowing the resolution of peptides having identical charges at a given pH. The selectivity can be manipulated by the addition of organic solvent to the mobile phases; this increases the retention of some peptides and decreases the retention of others. The retention in any given case may reflect a combination of steric factors and non-electrostatic interactions. Selectivity was complementary to that of reversed-phase chromatography (RPC) materials. Excellent purifications were obtained by sequential use of PolySULFOETHYL Aspartamide and RPC columns for purification of peptides from crude tissue extracts. The new cation exchanger is quite promising as a supplement to RPC for general peptide chromatography. PMID:2844843

  3. Transport of copper ammines through a cation-exchange membrane during electrodialysis

    SciTech Connect

    Kireeva, L.D.; Shaposhnik, V.A.; Sorokina, V.I.

    1987-09-10

    Extraction of copper ammine complexes from waste waters in electroplating technology and in production of cuprammonium fibers is an important problem and electrodialysis with ion-exchange membranes is the most promising method of solving it. The authors aim was to study transport of copper(II) ammines through a commercial cation-exchange membrane of the MK-40 type. The electrodialyzer consisted of five Plexiglas compartments separated in alternating order by MK-40 cation-exchange and MA-40 anion-exchange membranes. The authors studied the dependence of the transport of copper(II) ammine complexes on the current density at copper concentration 0.025 M in the desalination compartment and 0.15 M ammonia concentration. The experiments lead to the conclusion that electrodialysis of copper(II) ammine complexes is possible only at current densities below the limiting values and that the transport is accompanied by decrease of the formation function of the complexes both in the membrane and in the solution of the concentrate receiving compartment.

  4. Preparation and characterization of high capacity, strong cation-exchange fiber based adsorbents.

    PubMed

    Schwellenbach, Jan; Taft, Florian; Villain, Louis; Strube, Jochen

    2016-05-20

    Motivated by the demand for more economical capture and polishing steps in downstream processing of protein therapeutics, a novel strong cation-exchange chromatography stationary phase based on polyethylene terephthalate (PET) high surface area short-cut fibers is presented. The fiber surface is modified by grafting glycidyl methacrylate (GMA) via surface-initiated atom transfer radical polymerization (SI-ATRP) and a subsequent derivatization leading to sulfonic acid groups. The obtained cation-exchange fibers have been characterized and compared to commercially available resin and membrane based adsorbers. High volumetric static binding capacities for lysozyme (90mg/mL) and polyclonal human IgG (hIgG, 92mg/mL) were found, suggesting an efficient multi-layer binding within the grafted hydrogel layer. A packed bed of randomly orientated fibers has been tested for packing efficiency, permeability and chromatographic performance. High dynamic binding capacities for lysozyme (50mg/mL) and hIgG (54mg/mL) were found nearly independent of the bed-residence time, revealing a fast mass-transport mechanism. Height equivalent to a theoretical plate (HETP) values in the order of 0.1 cm and a peak asymmetry factor (AF) of 1.8 have been determined by tracer experiments. Additionally inverse size-exclusion chromatography (iSEC) revealed a bimodal structure within the fiber bed, consisting of larger transport channels, formed by the voidage between the fibers, and a hydrogel layer with porous properties. PMID:27106396

  5. Cation Exchange Synthesis and Unusual Resistive Switching Behaviors of Ag2Se Nanobelts.

    PubMed

    Guo, Zheng; Li, Min-Qiang; Liu, Jin-Huai; Huang, Xing-Jiu

    2015-12-16

    Ag2Se nanobelts are prepared through employing ZnSe nanobelts as templates via a facile cation exchange approach. The templates are derived from precursor ZnSe·0.5N2 H4 nanobelts, which are synthesized by a simple hydrothermal method. As-synthesized precursor nanobelts are with 200 nm in width and several hundreds of micrometers in length. Annealed in N2 , they are transformed into ZnSe nanobelts with preserving their initial morphology. Following with a complete replacement of Zn(2+) by Ag(+), Ag2Se nanobelts with single crystalline are obtained via a cation-exchange reaction. Combined with the Langmuir-Blodgett assembly technique, regular films of ZnSe nanobelts can be achieved on transparent glass substrates and Si wafers with interdigital Au electrode arrays. Further, the optical and electrical evolutions are investigated from ZnSe nanobelts to Ag2 Se nanobelts. Finally, the resistive switching characteristic are carefully explored for Ag2Se nanobelts regularly arranged on interdigital Au microelectrodes. The results indicate that it is analogous to complementary resistive switching behaviors, which is different from that of traditional two terminal devices about previously reported Ag2Se. In order to clarify this phenomenon, a possible mechanism has been proposed and indirectly demonstrated through in situ SEM (scanning electron microscropy) observation. PMID:26509434

  6. Some investigations on the radiation stability of a strongly acidic cation exchange resin

    NASA Astrophysics Data System (ADS)

    Dessouki, A. M.; Zahran, A. H.; Rabie, A. M.; Amer, S. I.

    The radiation-chemical stability of Merck Cation Exchanger I, a strongly acidic sulphonated cation exchanger of the polymerization type based on styrene-divinylbenze (DVB) copolymers was investigated. The radiation stability of the resin was assessed from the change in exchange capacity, loss in weight, change in swelling behaviour and formation of new exchange groups. The loss in capacity was 44 and 32% for resin specimens in the H +-form irradiated to 1000 Mrad in air and in vacuum, respectively. The Na +-form of the exchanger showed high resistance to radiation and the loss in capacity did not exceed 7% at a dose of 1000 Mrad. The loss in capacity was accompanied by a loss in weight and a decrease in the degree of swelling of the irradiated resin. The formation of new functional groups of the carboxylic and phenolic types was confirmed. The amount of these group increases with the increase in the integral dose. The amount of sulphuric acid formed as a result of irradiating the resin in the dry and moist states was determined. An increase in the moisture content of the resin resulted in a marked decrease in its radiation stability.

  7. Solubility and cation exchange in phosphate rock and saturated clinoptilolite mixtures

    NASA Technical Reports Server (NTRS)

    Allen, E. R.; Hossner, L. R.; Ming, D. W.; Henninger, D. L.

    1993-01-01

    Mixtures of zeolite and phosphate rock (PR) have the potential to provide slow-release fertilization of plants in synthetic soils by dissolution and ion-exchange reactions. This study was conducted to examine solubility and cation-exchange relationships in mixtures of PR and NH4- and K-saturated clinoptilolite (Cp). Batch-equilibration experiments were designed to investigate the effect of PR source, the proportion of exchangeable K and NH4, and the Cp to PR ratio on solution N, P, K, and Ca concentrations. The dissolution and cation-exchange reactions that occurred after mixing NH4- and K-saturated Cp with PR increased the solubility of the PR and simultaneously released NH4 and K into solution. The more reactive North Carolina (NC) PR rendered higher solution concentrations of NH4 and K when mixed with Cp than did Tennessee (TN) PR. Solution P concentrations for the Cp-NC PR mixture and the Cp-TN PR mixture were similar. Solution concentrations of N, P, K, and Ca and the ratios of these nutrients in solution varied predictably with the type of PR, the Cp/PR ratio, and the proportions of exchangeable K and NH4 on the Cp. Our research indicated that slow-release fertilization using Cp/PR media may provide adequate levels of N, P, and K to support plant growth. Solution Ca concentrations were lower than optimum for plant growth.

  8. Purification of urokinase by combined cation exchanger and affinity chromatographic cartridges.

    PubMed

    Hou, K C; Zaniewski, R

    1990-02-23

    Crude urokinase from human urine processed through foam flotation and ammonium sulfate precipitation containing 720 National Health Institute Committee on Thrombolytic Agents U/mg activity was purified by an SP cation exchanger followed by a zinc-chelated affinity chromatographic cartridge. The cartridges were of a radial-flow type formed by using acrylic and cellulose composite matrices. The high rigidity of the matrix structure permits fast flow of protein solutions (liters per minute) and thus allows processing of a large volume of crude urokinase under low operating pressures. A greater than six-fold increase in specific enzyme activity of urokinase was achieved by adsorbing and eluting 1 l of a 3 mg/ml crude urokinase solution on an SP cartridge. The eluent was further purified by passing through a zinc-chelated affinity cartridge to achieve greater than a eighteen-fold increase in urokinase specific activity. This report demonstrates the combined use of a cation exchanger with zinc-chelated chromatographic cartridges in purifying urokinase on a relatively large scale. The relationship between the amount of zinc chelated in the matrix to its effect on urokinase purification is also discussed. PMID:2329161

  9. Cation Exchange in Dynamic 3D Porous Magnets: Improvement of the Physical Properties.

    PubMed

    Grancha, Thais; Acosta, Alvaro; Cano, Joan; Ferrando-Soria, Jesús; Seoane, Beatriz; Gascon, Jorge; Pasán, Jorge; Armentano, Donatella; Pardo, Emilio

    2015-11-16

    We report two novel three-dimensional porous coordination polymers (PCPs) of formulas Li4{Mn4[Cu2(Me3mpba)2]3}·68H2O (2) and K4{Mn4[Cu2(Me3mpba)2]3}·69H2O (3) obtained-via alkali cation exchange in a single-crystal to single-crystal process-from the earlier reported anionic manganese(II)-copper(II) PCP of formula Na4{Mn4[Cu2(Me3mpba)2]3}·60H2O (1) [Me3mpba(4-) = N,N'-2,4,6-trimethyl-1,3-phenylenebis(oxamate)]. This postsynthetic process succeeds where the direct synthesis in solution from the corresponding building blocks fails and affords significantly more robust PCPs with enhanced magnetic properties [long-range 3D magnetic ordering temperatures for the dehydrated phases (1'-3') of 2.0 (1'), 12.0 (2'), and 20.0 K (3')]. Changes in the adsorptive properties upon postsynthetic exchange suggest that the nature, electrostatic properties, mobility, and location of the cations within the framework are crucial for the enhanced structural stability. Overall, these results further confirm the potential of postsynthetic methods (including cation exchange) to obtain PCPs with novel or enhanced physical properties while maintaining unaltered their open-framework structures. PMID:26492551

  10. Light-induced cation exchange for copper sulfide based CO2 reduction.

    PubMed

    Manzi, Aurora; Simon, Thomas; Sonnleitner, Clemens; Döblinger, Markus; Wyrwich, Regina; Stern, Omar; Stolarczyk, Jacek K; Feldmann, Jochen

    2015-11-11

    Copper(I)-based catalysts, such as Cu2S, are considered to be very promising materials for photocatalytic CO2 reduction. A common synthesis route for Cu2S via cation exchange from CdS nanocrystals requires Cu(I) precursors, organic solvents, and neutral atmosphere, but these conditions are not compatible with in situ applications in photocatalysis. Here we propose a novel cation exchange reaction that takes advantage of the reducing potential of photoexcited electrons in the conduction band of CdS and proceeds with Cu(II) precursors in an aqueous environment and under aerobic conditions. We show that the synthesized Cu2S photocatalyst can be efficiently used for the reduction of CO2 to carbon monoxide and methane, achieving formation rates of 3.02 and 0.13 μmol h(-1) g(-1), respectively, and suppressing competing water reduction. The process opens new pathways for the preparation of new efficient photocatalysts from readily available nanostructured templates. PMID:26479775

  11. Reducing the Cation Exchange Capacity of Lithium Clay to Form Better Dispersed Polymer-Clay Nanocomposites

    NASA Technical Reports Server (NTRS)

    Liang, Maggie

    2004-01-01

    Polymer-clay nanocomposites have exhibited superior strength and thermo- oxidative properties as compared to pure polymers for use in air and space craft; however, there has often been difficulty completely dispersing the clay within the matrices of the polymer. In order to improve this process, the cation exchange capacity of lithium clay is first lowered using twenty-four hour heat treatments of no heat, 130 C, 150 C, or 170 C to fixate the lithium ions within the clay layers so that they are unexchangeable. Generally, higher temperatures have generated lower cation exchange capacities. An ion exchange involving dodecylamine, octadecylamine, or dimethyl benzidine (DMBZ) is then employed to actually expand the clay galleries. X-ray diffraction and transmission electron microscopy can be used to determine whether the clay has been successfully exfoliated. Finally, resins of DMBZ with clay are then pressed into disks for characterization using dynamic mechanical analyzer and oven- aging techniques in order to evaluate their glass transition, modulus strength, and thermal-oxidative stability in comparison to neat DMBZ. In the future, they may also be tested as composites for flexural and laminar shear strength.

  12. Cu₂Se and Cu Nanocrystals as Local Sources of Copper in Thermally Activated In Situ Cation Exchange.

    PubMed

    Casu, Alberto; Genovese, Alessandro; Manna, Liberato; Longo, Paolo; Buha, Joka; Botton, Gianluigi A; Lazar, Sorin; Kahaly, Mousumi Upadhyay; Schwingenschloegl, Udo; Prato, Mirko; Li, Hongbo; Ghosh, Sandeep; Palazon, Francisco; De Donato, Francesco; Mozo, Sergio Lentijo; Zuddas, Efisio; Falqui, Andrea

    2016-02-23

    Among the different synthesis approaches to colloidal nanocrystals, a recently developed toolkit is represented by cation exchange reactions, where the use of template nanocrystals gives access to materials that would be hardly attainable via direct synthesis. Besides, postsynthetic treatments, such as thermally activated solid-state reactions, represent a further flourishing route to promote finely controlled cation exchange. Here, we report that, upon in situ heating in a transmission electron microscope, Cu2Se or Cu nanocrystals deposited on an amorphous solid substrate undergo partial loss of Cu atoms, which are then engaged in local cation exchange reactions with Cu "acceptor" phases represented by rod- and wire-shaped CdSe nanocrystals. This thermal treatment slowly transforms the initial CdSe nanocrystals into Cu(2-x)Se nanocrystals, through the complete sublimation of Cd and the partial sublimation of Se atoms. Both Cu "donor" and "acceptor" particles were not always in direct contact with each other; hence, the gradual transfer of Cu species from Cu2Se or metallic Cu to CdSe nanocrystals was mediated by the substrate and depended on the distance between the donor and acceptor nanostructures. Differently from what happens in the comparably faster cation exchange reactions performed in liquid solution, this study shows that slow cation exchange reactions can be performed at the solid state and helps to shed light on the intermediate steps involved in such reactions. PMID:26816347

  13. Cu2Se and Cu Nanocrystals as Local Sources of Copper in Thermally Activated In Situ Cation Exchange

    PubMed Central

    2016-01-01

    Among the different synthesis approaches to colloidal nanocrystals, a recently developed toolkit is represented by cation exchange reactions, where the use of template nanocrystals gives access to materials that would be hardly attainable via direct synthesis. Besides, postsynthetic treatments, such as thermally activated solid-state reactions, represent a further flourishing route to promote finely controlled cation exchange. Here, we report that, upon in situ heating in a transmission electron microscope, Cu2Se or Cu nanocrystals deposited on an amorphous solid substrate undergo partial loss of Cu atoms, which are then engaged in local cation exchange reactions with Cu “acceptor” phases represented by rod- and wire-shaped CdSe nanocrystals. This thermal treatment slowly transforms the initial CdSe nanocrystals into Cu2–xSe nanocrystals, through the complete sublimation of Cd and the partial sublimation of Se atoms. Both Cu “donor” and “acceptor” particles were not always in direct contact with each other; hence, the gradual transfer of Cu species from Cu2Se or metallic Cu to CdSe nanocrystals was mediated by the substrate and depended on the distance between the donor and acceptor nanostructures. Differently from what happens in the comparably faster cation exchange reactions performed in liquid solution, this study shows that slow cation exchange reactions can be performed at the solid state and helps to shed light on the intermediate steps involved in such reactions. PMID:26816347

  14. Nano-Composite Material Development for 3-D Printers

    SciTech Connect

    Satches, Michael Randolph

    2015-12-01

    Graphene possesses excellent mechanical properties with a tensile strength that may exceed 130 GPa, excellent electrical conductivity, and good thermal properties. Future nano-composites can leverage many of these material properties in an attempt to build designer materials for a broad range of applications. 3-D printing has also seen vast improvements in recent years that have allowed many companies and individuals to realize rapid prototyping for relatively low capital investment. This research sought to create a graphene reinforced, polymer matrix nano-composite that is viable in commercial 3D printer technology, study the effects of ultra-high loading percentages of graphene in polymer matrices and determine the functional upper limit for loading. Loadings varied from 5 wt. % to 50 wt. % graphene nanopowder loaded in Acrylonitrile Butadiene Styrene (ABS) matrices. Loaded sample were characterized for their mechanical properties using three point bending, tensile tests, as well as dynamic mechanical analysis.

  15. Studies on structural properties of clay magnesium ferrite nano composite

    NASA Astrophysics Data System (ADS)

    Kaur, Manpreet; Singh, Mandeep; Jeet, Kiran; Kaur, Rajdeep

    2015-08-01

    Magnesium ferrite-bentonite clay composite was prepared by sol-gel combustion method employing citric acid as complexing agent and fuel. The effect of clay on the structural properties was studied with X-ray diffraction (XRD), Fourier transform infrared (FT-IR) Spectroscopy, Scanning electron microscopy (SEM), SEM- Energy dispersive Spectroscope (EDS) and BET surface area analyzer. Decrease in particle size and density was observed on addition of bentonite clay. The BET surface area of nano composite containing just 5 percent clay was 74.86 m2/g. Whereas porosity increased from 40.5 per cent for the pure magnesium ferrite to 81.0 percent in the composite showing that nano-composite has potential application as an adsorbent.

  16. Studies on structural properties of clay magnesium ferrite nano composite

    SciTech Connect

    Kaur, Manpreet Singh, Mandeep; Jeet, Kiran Kaur, Rajdeep

    2015-08-28

    Magnesium ferrite-bentonite clay composite was prepared by sol-gel combustion method employing citric acid as complexing agent and fuel. The effect of clay on the structural properties was studied with X-ray diffraction (XRD), Fourier transform infrared (FT-IR) Spectroscopy, Scanning electron microscopy (SEM), SEM- Energy dispersive Spectroscope (EDS) and BET surface area analyzer. Decrease in particle size and density was observed on addition of bentonite clay. The BET surface area of nano composite containing just 5 percent clay was 74.86 m{sup 2}/g. Whereas porosity increased from 40.5 per cent for the pure magnesium ferrite to 81.0 percent in the composite showing that nano-composite has potential application as an adsorbent.

  17. Electrodialysis of Sulfuric Acid with Cation-Exchange Membranes Prepared by Electron-Beam-Induced Graft Polymerization

    NASA Astrophysics Data System (ADS)

    Asari, Yuki; Shoji, Nobuyoshi; Miyoshi, Kazuyoshi; Umeno, Daisuke; Saito, Kyoichi

    Strongly acidic cation-exchange membranes were prepared by the electron-beam-induced graft polymerization of glycidyl methacrylate onto a high-density polyethylene film with a thickness of 35 μm and the subsequent conversion of the resulting epoxy group into a sulfonic acid group. The resulting cation-exchange membranes with various ion-exchange capacities or sulfonic acid group densities ranging from 1.9 to 2.7 mmol/g were applied to the enrichment of 0.50 mol/L sulfuric acid by electrodialysis. Concentrated sulfuric acids at concentrations of 1.4 to 2.9 mol/L were obtained in the concentrate chamber during the electrodialysis operated at 30 mA/cm2 and 298 K, using a pair of this cation-exchange membrane and a commercially available anion-exchange membrane.

  18. Fast doping of Cu into ZnSe NCs by hydrazine promoted cation exchange in aqueous solution at room temperature.

    PubMed

    Shao, Haibao; Wang, Chunlei; Xu, Shuhong; Wang, Zhuyuan; Yin, Haihong; Cui, Yiping

    2015-03-01

    Controllable doping is an effective way of tuning the properties of semiconductor nanocrystals (NCs). In this work, a simple strategy of fast doping Cu ions into ZnSe NCs under ambient conditions was proposed. The principle of doping is based on hydrazine (N2H4) promoted cation exchange reaction. By direct addition of Cu ion stock solution into the preformed ZnSe NCs, Cu doped ZnSe NCs can be obtained. Furthermore, the emission of doped NCs can be tuned by changing the amount of impurity ion addition. The cation exchange reaction is facilitated by three factors: 1) N2H4 addition, 2) fast impurity ions, and 3) partial stabilizer removal. The proposed cation exchange reaction in aqueous solution could be an alternate route for NC doping as well as synthesis of ionic NCs. PMID:25605441

  19. Influence of the Ion Coordination Number on Cation Exchange Reactions with Copper Telluride Nanocrystals.

    PubMed

    Tu, Renyong; Xie, Yi; Bertoni, Giovanni; Lak, Aidin; Gaspari, Roberto; Rapallo, Arnaldo; Cavalli, Andrea; Trizio, Luca De; Manna, Liberato

    2016-06-01

    Cu2-xTe nanocubes were used as starting seeds to access metal telluride nanocrystals by cation exchanges at room temperature. The coordination number of the entering cations was found to play an important role in dictating the reaction pathways. The exchanges with tetrahedrally coordinated cations (i.e., with coordination number 4), such as Cd(2+) or Hg(2+), yielded monocrystalline CdTe or HgTe nanocrystals with Cu2-xTe/CdTe or Cu2-xTe/HgTe Janus-like heterostructures as intermediates. The formation of Janus-like architectures was attributed to the high diffusion rate of the relatively small tetrahedrally coordinated cations, which could rapidly diffuse in the Cu2-xTe NCs and nucleate the CdTe (or HgTe) phase in a preferred region of the host structure. Also, with both Cd(2+) and Hg(2+) ions the exchange led to wurtzite CdTe and HgTe phases rather than the more stable zinc-blende ones, indicating that the anion framework of the starting Cu2-xTe particles could be more easily deformed to match the anion framework of the metastable wurtzite structures. As hexagonal HgTe had never been reported to date, this represents another case of metastable new phases that can only be accessed by cation exchange. On the other hand, the exchanges involving octahedrally coordinated ions (i.e., with coordination number 6), such as Pb(2+) or Sn(2+), yielded rock-salt polycrystalline PbTe or SnTe nanocrystals with Cu2-xTe@PbTe or Cu2-xTe@SnTe core@shell architectures at the early stages of the exchange process. In this case, the octahedrally coordinated ions are probably too large to diffuse easily through the Cu2-xTe structure: their limited diffusion rate restricts their initial reaction to the surface of the nanocrystals, where cation exchange is initiated unselectively, leading to core@shell architectures. Interestingly, these heterostructures were found to be metastable as they evolved to stable Janus-like architectures if annealed at 200 °C under vacuum. PMID:27177274

  20. Time-Resolved Structural Analysis of Cation Exchange Reactions in Birnessite Using Synchrotron XRD

    NASA Astrophysics Data System (ADS)

    Lopano, C. L.; Heaney, P. J.; Post, J. E.; Hanson, J. C.; Lee, Y.; Komarneni, S.

    2002-12-01

    Birnessite ((Na,Ca,Mn2+) Mn7O142.8H2O) is a layered Mn-oxide with a 7.2Å spacing between the Mn octahedral sheets. Since birnessite is an abundant phase in soils, desert varnishes, and ocean nodules, it plays a significant role in soil and groundwater chemistry. Experiments by Golden et al. (1986,1987) have demonstrated that Na-buserite (hydrated birnessite) readily exchanges Na+ for a variety of other cations, including K+, Mg2+, Ca2+, Ba2+, Ni2+, and Sr2+. In light of its high cation exchange capacity, birnessite is industrially important for ion and molecular sieves and cathodic materials. In addition, birnessite serves as a precursor in the synthesis of todorokite, which has a 3x3 tunnel structure and is used as an octahedral sieve. We monitored cation-exchange reactions in birnessite by time-resolved X-ray powder diffraction with a simple flow-through cell at the National Synchrotron Light Source. The flow-through cell was developed by Lee and Parise at SUNY-Stony Brook, and this work represents its first application to Mn oxides. A series of synthetic Na-birnessite samples were saturated with chloride solutions containing dissolved K+, Mg2+, and Ba2+, ranging from 0.1M to 0.001M. Powder X-ray diffraction patterns were collected every ~ 3 minutes. The synchrotron experiments revealed that complete cation exchange occurs within three hours, and significant modifications of the arrangements of interlayer cations and water molecules accompany the exchange. Specifically, the replacement of Na by Mg resulted in the continuous growth of a discrete buserite-like phase with a 10Å layer spacing, while replacement of Na by K and Ba retained the 7Å spacing. K replacement of Na resulted in gradually decreasing peak intensity and peak merging. The Ba exchange yielded an abrupt decrease in diffraction intensities followed by a more gradual lattice change over the last 2 hours. Rietveld analysis led to the first determination of the structure of Ba-birnessite in space

  1. Salbutamol versus cation-exchange resin (kayexalate) for the treatment of nonoliguric hyperkalemia in preterm infants.

    PubMed

    Yaseen, Hakam; Khalaf, Mona; Dana, Ahmed; Yaseen, Noha; Darwich, Maha

    2008-03-01

    Our objective was to compare the efficacy and safety of rectal cation-exchange resin (Kayexalate) versus salbutamol infusion for the treatment of nonoliguric hyperkalemia (NOHK) in preterm infants. Data of all neonates born with NOHK during the study period of 6 years and 8 months were recorded. Diagnostic criteria of NOHK included serum potassium (SK) concentration > or = 7 mmol/L during the first 72 hours of life with urine output > or = 1 mL/kg/hour. This before-after study was divided according to the date of admission; the first 15 patients were treated with Kayexalate enema 1 g/kg every 4 hours, and the remaining 30 patients were treated with intravenous salbutamol infusion as 4 mug/kg every 4 hours. Treatment discontinued when SK became < 6 mmol/L. SK was measured every 4 hours. Daily urine was collected. Fluid intake and output, serum electrolytes, urea, creatinine, and glucose concentrations were obtained in all infants every 12 hours. All infants were observed with a cardiorespiratory monitor and oxygen saturation and blood pressure measurements. Perinatal characteristics in both groups were comparable. Mean gestational age was 26 and 28 weeks for salbutamol and Kayexalate, respectively. The peak of SK ranged between 7 and 9.3 mmol/L in the Kayexalate group and between 7 and 8.7 mmol/L in the salbutamol group ( P = 0.64). At 12 hours of treatment, SK became normal in only 4 patients (26%) in the Kayexalate group compared with 18 patients (60%) in the salbutamol group ( P = 0.003). The number of doses of Kayexalate administration was significantly higher than the doses of salbutamol ( P = 0.003). No significant side effects were detected in the salbutamol-treated infants. In contrast, there were two cases of severe ventricular tachycardia and one case of intestinal obstruction in the cation-exchange resin group. We concluded that salbutamol infusion is more effective with faster action and safer than cation-exchange resin (Kayexalate) for the treatment of

  2. Continuous process of preparation of n-butyl(meth)acrylate by esterification of (meth)acrylic acid by butanol on thermostable sulfo-cation exchanger

    SciTech Connect

    Zheleznaya, L.L.; Karakhanov, R.A.; Lunin, A.F.; Magadov, R.S.; Meshcheryakov, S.V.; Mkrtychan, V.R.; Fomin, V.A.

    1987-11-10

    The authors propose an effective thermostable sulfo-cation exchanger based on polymers with a system of conjugated bonds, sulfopolyphenylene ketone (SPP) differing from the known cation exchangers by the high thermostability (up to 250/sup 0/C), and also having the effect of the stabilization of the double bond in unsaturated monomers. The combination of inhibiting and cation exchange properties makes it also possible to use these sulfo-cation exchangers in the processes of esterification of (meth)acrylic acids by alcohols without addition of special inhibitors. The SPP catalyst was tested in esterification processes of acrylic an methacrylic acid by butanol at a pilot plant.

  3. Local reactivity descriptors to predict the strength of Lewis acid sites in alkali cation-exchanged zeolites

    NASA Astrophysics Data System (ADS)

    Deka, Ramesh Ch.; Kinkar Roy, Ram; Hirao, Kimihiko

    2004-05-01

    Lewis acidity of alkali cation-exchanged zeolite is studied using local reactivity descriptors based on hard-soft acid-base (HSAB) concept. The local softness for nucleophilic attack ( sx+), local softness for electrophilic attack ( sx-) and their ratio, which is called `relative electrophilicity' ( sx+/ sx-), are calculated for the exchanged cations and Lewis acidity of the cations is found to decrease in the order: Li + > Na + > K + > Rb + > Cs +. Calculated blue shift of CO vibrational frequency (Δ ν) and interaction energy of CO molecule with alkali cation-exchanged zeolite clusters vary linearly with sx+/ sx- values.

  4. Synthesis of ordered mesoporous crystalline CuS and Ag2S materials via cation exchange reaction

    NASA Astrophysics Data System (ADS)

    Wang, Jun; Xu, Weiming; Bao, Haifeng; Shi, Yifeng

    2015-02-01

    Cation exchange reaction is a strong tool for the synthesis of new ionic nanomaterials. Most of them are isolated nanoparticles with simple geometric features, such as nanodots, nanorods and nanospheres. In this work, we demonstrated that ordered mesoporous CdS with a complex cubic Ia3d gyroidal 3D bicontinuous porous structure and large particle size can be successfully converted to crystalline CuS and Ag2S materials via cation exchange reaction without destroying the well-defined nanostructure. The change in crystal structure is an important factor for a successful conversion when the reaction is carried out without the presence of a silica template. In addition, the cation exchange reaction is sufficient for a complete compositional conversion, even when the mesostructured CdS precursor is embedded inside a mesoporous silica matrix. Our results indicate that cation exchange reaction may be applied to highly complex nanostructures with extremely large particle sizes.Cation exchange reaction is a strong tool for the synthesis of new ionic nanomaterials. Most of them are isolated nanoparticles with simple geometric features, such as nanodots, nanorods and nanospheres. In this work, we demonstrated that ordered mesoporous CdS with a complex cubic Ia3d gyroidal 3D bicontinuous porous structure and large particle size can be successfully converted to crystalline CuS and Ag2S materials via cation exchange reaction without destroying the well-defined nanostructure. The change in crystal structure is an important factor for a successful conversion when the reaction is carried out without the presence of a silica template. In addition, the cation exchange reaction is sufficient for a complete compositional conversion, even when the mesostructured CdS precursor is embedded inside a mesoporous silica matrix. Our results indicate that cation exchange reaction may be applied to highly complex nanostructures with extremely large particle sizes. Electronic supplementary

  5. Phenolic cation exchange resin material for recovery of cesium and strontium

    DOEpatents

    Ebra, Martha A.; Wallace, Richard M.

    1983-01-01

    A phenolic cation exchange resin with a chelating group has been prepared by reacting resorcinol with iminodiacetic acid in the presence of formaldehyde at a molar ratio of about 1:1:6. The material is highly selective for the simultaneous recovery of both cesium and strontium from aqueous alkaline solutions, such as, aqueous alkaline nuclear waste solutions. The organic resins are condensation polymers of resorcinol and formaldehyde with attached chelating groups. The column performance of the resins compares favorably with that of commercially available resins for either cesium or strontium removal. By combining Cs.sup.+ and Sr.sup.2+ removal in the same bed, the resins allow significant reduction of the size and complexity of facilities for processing nuclear waste.

  6. Controlled methyl-esterification of pectin catalyzed by cation exchange resin.

    PubMed

    Peng, Xiaoxia; Yang, Guang; Fan, Xingchen; Bai, Yeming; Ren, Xiaomeng; Zhou, Yifa

    2016-02-10

    This study developed a new method to methyl-esterify pectin using a cation exchange resin. Homogalacturonan (HG)-type pectin (WGPA-3-HG) and rhamnogalacturonan (RG)-I-type pectin (AHP-RG) obtained from the roots of Panax ginseng and sunflower heads, respectively, were used as models. Compared to commonly used methyl-esterification methods that use either methyl iodide or acidified methanol, the developed method can methyl-esterify both HG- and RG-I-type pectins without degrading their structures via β-elimination or acid hydrolysis. In addition, by modifying reaction conditions, including the mass ratio of resin to pectin, reaction time, and temperature, the degree of esterification can be controlled. Moreover, the resin and methanol can be recycled to conserve resources, lower costs, and reduce environmental pollution. This new methodology will be highly useful for industrial esterification of pectin. PMID:26686175

  7. Kaolins: sources of differences in cation-exchange capacities and cesium retention

    SciTech Connect

    Lim. C.H.; Jackson, M.L.; Koons, R.D.; Helmke, P.A.

    1980-01-01

    Seven kaolins from Georgia (southeastern USA), ranging from high to low commercial grade, were characterized by x-ray powder diffraction and chemical techniques to establish that the variation in quality was caused by impurities. The Ca and Cs cation-exchange capacities (CEC) varied from 2.67 to 8.17 and from 3.29 to 8.77 meq/100 g, respectively. The external surface CEC of kaolinite ranged from 0 to 1 meq/100 g. The Cs-retention capacity (0.19 to 1.14 meq/100 g) was closely related to Cs-measured vermiculite content and this content plus specific surface mica content. The Cs retention appeared to be primarily related to the presence of interlayer wedges at mica/vermiculite XY interfaces.

  8. Pullulan Production by Aureobasidium pullulans ATCC 201253 Cells Adsorbed onto Cellulose Anion and Cation Exchangers

    PubMed Central

    West, Thomas P.

    2012-01-01

    The anion exchanger phosphocellulose and the cation exchanger triethylaminoethyl cellulose were used to immobilize cells of the fungus Aureobasidium pullulans ATCC 201253 and the adsorbed cells were subsequently investigated for their ability to produce the polysaccharide pullulan using batch fermentation. The cells adsorbed on the triethylaminoethyl cellulose at pH 7.5 produced higher pullulan levels than those cells immobilized on phosphocellulose at pH 4.0 for 2 cycles of 168 h at 30 °C. Relative to the initial cycle of 168 h, pullulan production by the cells immobilized on the triethylaminoethyl cellulose decreased slightly after 168 h of the second production cycle while pullulan production by the phosphocellulose-immobilized cells remained about the same after 168 h of the second production cycle. PMID:23762749

  9. A New Cation-Exchange Method for Accurate Field Speciation of Hexavalent Chromium

    USGS Publications Warehouse

    Ball, James W.; McCleskey, R. Blaine

    2003-01-01

    A new cation-exchange method for field speciation of Cr(VI) has been developed to meet present stringent regulatory standards and to overcome the limitations of existing methods. The new method allows measurement of Cr(VI) concentrations as low as 0.05 micrograms per liter, storage of samples for at least several weeks prior to analysis, and use of readily available analytical instrumentation. The sensitivity, accuracy, and precision of the determination in waters over the pH range of 2 to 11 and Fe concentrations up to 1 milligram per liter are equal to or better than existing methods such as USEPA method 218.6. Time stability of preserved samples is a significant advantage over the 24-hour time constraint specified for USEPA method 218.6.

  10. Quantitative separation of gallium from other elements by cation-exchange chromatography

    SciTech Connect

    van der Walt, T.N.; Strelow, F.W.E.

    1983-02-01

    Trace amounts and up to 1.5 mg of gallium can be separated from up to gram amounts of Al, Cd, Cu, In, Mn, Ni, Pb, U(VI), and many other elements by eluting these elements with 8.0 M hydrochloric acid from a column containing 13.0 mL (3.0 g) of AG 50W-X4 cation-exchange resin of 100-200 mesh particle size in the H-form. Gallium can be separated from up to 2 g of iron(II) and up to 10 mg of scandium by eluting the iron with 8.0 M hydrochloric acid containing 0.30% titanium(III) chloride and eluting the scandium with 7.0 M hydrochloric acid. The retained gallium is effectively eluted with 2.5 M hydrochloric acid. Separations are sharp and quantitative. 5 figures, 3 tables.

  11. Cation–cation interactions and cation exchange in a series of isostructural framework uranyl tungstates

    SciTech Connect

    Balboni, Enrica; Burns, Peter C.

    2014-05-01

    The isotypical compounds (UO{sub 2}){sub 3}(WO{sub 6})(H{sub 2}O){sub 5} (1), Ag(UO{sub 2}){sub 3}(WO{sub 6})(OH)(H{sub 2}O){sub 3} (2), K(UO{sub 2}){sub 3}(WO{sub 6})OH(H{sub 2}O){sub 4} (3), Rb(UO{sub 2}){sub 3}(WO{sub 6})(OH)(H{sub 2}O){sub 3.5} (4), and Cs(UO{sub 2}){sub 3}(WO{sub 6})OH(H{sub 2}O){sub 3} (5) were synthesized, characterized, and their structures determined. Each crystallizes in space group Cc. (1): a=12.979 (3), b=10.238 (2), c=11.302 (2), β=102.044 (2); (2): a=13.148 (2), b=9.520 (1), c=11.083 (2), β=101.568 (2); (3): a=13.111 (8), b=9.930 (6), c=11.242 (7), β=101.024 (7); (4): a=12.940 (2), b=10.231 (2), c=11.259(2), β=102.205 (2); (5): a=12.983 (3), b=10.191 (3), c=11.263 (4), β=101.661 (4). Compounds 1–5 are a framework of uranyl and tungsten polyhedra containing cation–cation interactions. The framework has three symmetrically distinct U(VI) cations, one tungsten, sixteen to eighteen oxygen atoms, and in 2–5, one monovalent cation. Each atom occupies a general position. Each U(VI) cation is present as a typical (UO{sub 2}){sup 2+} uranyl ion in an overall pentagonal bipyramidal coordination environment. Each pentagonal bipyramid shares two equatorial edges with two other pentagonal bipyramids, forming a trimer. Trimers are connected into chains by edge-sharing with WO{sub 6} octahedra. Chains are linked through cation–cation interactions between two symmetrically independent uranyl ions. This yields a remarkably complex system of intersecting channels that extend along [0 0 1] and [−1 1 0]. The cation exchange properties of 2 and 3 were characterized at room temperature and at 140 °C. - Graphical abstract: Chains of uranium and tungsten polyhedra are connected into a three dimensional framework by cation–cation interactions occurring between two symmetrically independent uranyl pentagonal bipyramids. Monovalent cations present in channels within the structure can be exchanged by room temperature or mild hydrothermal

  12. Phenolic cation-exchange resin material for recovery of cesium and strontium. [Patent application

    DOEpatents

    Ebra, M.A.; Wallace, R.M.

    1982-05-05

    A phenolic cation exchange resin with a chelating group has been prepared by reacting resorcinol with iminodiacetic acid in the presence of formaldehyde at a molar ratio of about 1:1:6. The material is highly selective for the simultaneous recovery of both cesium and strontium from aqueous alkaline solutions, such as, aqueous alkaline nuclear wate solutions. The organic resins are condensation polymers of resorcinol and formaldehyde with attached chelating groups. The column performance of the resins compares favorably with that of commercially available resins for either cesium or strontium removal. By combining Cs/sup +/ and Sr/sup 2 +/ removal in the same bed, the resins allow significant reduction of the size and complexity of facilities for processing nuclear waste.

  13. New cation-exchange material based on a sulfonated 3,4-ethylenedioxythiophene monomer

    NASA Astrophysics Data System (ADS)

    Stéphan, O.; Schottland, P.; Le Gall, P.-Y.; Chevrot, C.

    1998-06-01

    The electrochemical oxidation, in aqueous medium, of a 3,4-ethylenedioxythiophene monomer functionalized by a sulfonate group exhibiting cation-exchange properties, allows the synthesis of a new type of water-soluble material. In order to synthesize in water, by oxidative electropolymerization, polymer films of controlled thickness containing attached sulfonate groups, we have investigated the polymerization of the functionalized monomer in the presence of the unsubstituted one without supporting electrolyte. Using an equimolar mixture (0.01 mol/l) of both monomers, copolymers exhibiting cation exchange abilities have been synthesized. As an example, th easy incorporation of hexaamine-ruthenium(III) into one of these copolymers is briefly reported. L'oxydation électrochimique en milieu aqueux d'un monomère de type 3,4- éthylènedioxythiophène fonctionnalisé par un groupement sulfonate permet d'envisager la synthèse d'un nouveau type de polymère hydrosoluble. Afin d'obtenir électrochimiquement en milieu aqueux, un film de polymère d'épaisseur contrôlée contenant des groupements sulfonates, nous avons evisagé de polymériser ce monomère en présence de son homologue non substitué. En partant d'un mélange équimolaire (0.01 mol/l) des deux monomères et en l'absence d'électrolyte support, nous avons synthétisé un matériau possédant des propriétés d'échange de cations. A titre d'exemple, nous présentons brièvement l'incorporation d'un complexe hexaaminé du ruthénium(III) dans un de ces copolymères.

  14. Synthesis and properties of a cation exchange resin prepared by the pyrolysis of starch in the presence of phytic acid

    SciTech Connect

    Lehrfeld, J.

    1995-12-01

    A material having cation exchange and adsorption properties was prepared by the controlled pyrolysis of starch in the presence of a commercial phytic acid solution. Resins can be prepared with binding capacities of 0.7-5.7 meq/g. These resins also have the ability to remove atrazine from aqueous solutions.

  15. Production of U{sub 3}O{sub 8} Using Macroporous Sulfonate Cation Exchange Resins in the Bead Form

    SciTech Connect

    Mosley, W.C.

    2001-08-16

    The use of cation exchange resin to product U{sub 3}O{sub 8} suitable for powder metallurgy fabrication of reactor fuel tubes with Al-U{sub 3}O{sub 8} cores is being investigated. This report presents the results of those studies.

  16. Solid-solid phase transformations induced through cation exchange and strain in 2D heterostructured copper sulfide nanocrystals.

    PubMed

    Ha, Don-Hyung; Caldwell, Andrew H; Ward, Matthew J; Honrao, Shreyas; Mathew, Kiran; Hovden, Robert; Koker, Margaret K A; Muller, David A; Hennig, Richard G; Robinson, Richard D

    2014-12-10

    We demonstrate dual interface formation in nanocrystals (NCs) through cation exchange, creating epitaxial heterostructures within spherical NCs. The thickness of the inner-disk layer can be tuned to form two-dimensional (2D), single atomic layers (<1 nm). During the cation exchange reaction from copper sulfide to zinc sulfide (ZnS), we observe a solid-solid phase transformation of the copper sulfide phase in heterostructured NCs. As the cation exchange reaction is initiated, Cu ions replaced by Zn ions at the interfaces are accommodated in intrinsic Cu vacancy sites present in the initial roxbyite (Cu1.81S) phase of copper sulfide, inducing a full phase transition to djurleite (Cu1.94S)/low chalcocite (Cu2S), a more thermodynamically stable phase than roxbyite. As the reaction proceeds and reduces the size of the copper sulfide layer, the epitaxial strain at the interfaces between copper sulfide and ZnS increases and is maximized for a copper sulfide disk ∼ 5 nm thick. To minimize this strain energy, a second phase transformation occurs back to the roxbyite phase, which shares a similar sulfur sublattice to wurtzite ZnS. The observation of a solid-solid phase transformation in our unique heterostructured NCs provides a new pathway to control desired phases and an insight into the influence of cation exchange on nanoscale phase transitions in heterostructured materials. PMID:25337657

  17. Quantification of unsaturated-zone alteration and cation exchange in zeolitized tuffs at Yucca Mountain, Nevada, USA

    NASA Astrophysics Data System (ADS)

    Vaniman, David T.; Chipera, Steve J.; Bish, David L.; Carey, J. William; Levy, Schön S.

    2001-10-01

    Zeolitized horizons in the unsaturated zone (UZ) at Yucca Mountain, Nevada, USA, are an important component in concepts for a high-level nuclear waste repository at this site. The use of combined quantitative X-ray diffraction and geochemical analysis allows measurement of the chemical changes that accompanied open-system zeolitization at Yucca Mountain. This approach also provides measures of the extent of chemical migration that has occurred in these horizons as a result of subsequent cation exchange. Mass-balance analysis of zeolitized horizons with extensive cation exchange (drill hole UZ-16) and with only minimal cation exchange (drill hole SD-9) shows that Al is essentially immobile. Although zeolitization occurred in an open system, the mass transfer of constituents other than water is relatively small in initial zeolitization, in contrast to the larger scales of cation exchange that can occur after zeolites have formed. Cation exchange in the clinoptilolite ± mordenite zeolitized horizons is seen in downward-diminishing concentration gradients of Ca, Mg, and Sr exchanged for Na and (to lesser extent) K. Comparison with data from drill hole SD-7, which has multiple zeolitized horizons above the water table, shows that the upper horizons accumulate Ca, Mg, and Sr to such an extent that transport of these elements to the deepest UZ zeolitized horizon can be blocked. Quantitative analysis of zeolite formation yields insight into processes that are implied from laboratory studies and modeling efforts but are otherwise unverified at the site. Such analysis also yields information not provided by or contradicted by some models of flow and transport. The results include the following: (1) evidence of effective downward flow through zeolitic horizons despite the low permeability of these horizons, (2) evidence that alkaline-earth elements accumulated by zeolites are mostly derived from eolian materials in surface soils, (3) validation of the very effective

  18. Assessing the role of cation exchange in controlling groundwater chemistry during fluid mixing in fractured granite at Aspo, Sweden

    SciTech Connect

    Viani, B.E.; Bruton, C.J.

    1996-06-01

    Geochemical modeling was used to simulate the mixing of dilute shallow groundwater with deeper more saline groundwater in the fractured granite of the Redox Zone at the Aespoe underground Hard Rock Laboratory (HRL). Fluid mixing simulations were designed to assess the role that cation exchange plays in controlling the composition of fluids entering the HRL via fracture flow. Mixing simulations included provision for the effects of mineral precipitation and cation exchange on fluid composition. Because the predominant clay mineral observed in fractures in the Redox Zone has been identified as illite or mixed layer illite smectite, an exchanger with the properties of illite was used to simulate cation exchange. Cation exchange on illite was modeled using three exchange sites, a planar or basal plane site with properties similar to smectite, and two edge sites that have very high affinities for K, Rb, and Cs. Each site was assumed to obey an ideal Vanselow exchange model, and exchange energies for each site were taken from the literature. The predicted behaviors of Na, Ca, and Mg during mixing were similar to those reported in a previous study in which smectite was used as the model for the exchanger. The trace elements Cs and Rb were predicted to be strongly associated with the illite exchanger, and the predicted concentrations of Cs in fracture fill were in reasonable agreement with reported chemical analyses of exchangeable Cs in fracture fill. The results of the geochemical modeling suggest that Na, Ca, and Sr concentrations in the fluid phase may be controlled by cation exchange reactions that occur during mixing, but that Mg appears to behave conservatively. There is currently not enough data to make conclusions regarding the behavior of Cs and Rb.

  19. Bandgap tunable colloidal Cu-based ternary and quaternary chalcogenide nanosheets via partial cation exchange

    NASA Astrophysics Data System (ADS)

    Ramasamy, Parthiban; Kim, Miri; Ra, Hyun-Soo; Kim, Jinkwon; Lee, Jong-Soo

    2016-04-01

    Copper based ternary and quaternary semiconductor nanostructures are of great interest for the fabrication of low cost photovoltaics. Although well-developed syntheses are available for zero dimensional (0D) nanoparticles, colloidal synthesis of two dimensional (2D) nanosheets remains a big challenge. Here we report, for the first time, a simple and reproducible cation exchange approach for 2D colloidal Cu2GeSe3, Cu2ZnGeSe4 and their alloyed Cu2GeSxSe3-x, Cu2ZnGeSxSe4-x nanosheets using pre-synthesized Cu2xSe nanosheets as a template. A mechanism for the formation of Cu2-xSe nanosheets has been studied in detail. In situ oxidation of Cu+ ions to form a CuSe secondary phase facilitates the formation of Cu2-xSe NSs. The obtained ternary and quaternary nanosheets have average lateral size in micrometers and thickness less than 5 nm. This method is general and can be extended to produce other important ternary semiconductor nanosheets such as CuIn1-xGaxSe2. The optical band gap of these nanosheets is tuned from 1 to 1.48 eV, depending on their composition.Copper based ternary and quaternary semiconductor nanostructures are of great interest for the fabrication of low cost photovoltaics. Although well-developed syntheses are available for zero dimensional (0D) nanoparticles, colloidal synthesis of two dimensional (2D) nanosheets remains a big challenge. Here we report, for the first time, a simple and reproducible cation exchange approach for 2D colloidal Cu2GeSe3, Cu2ZnGeSe4 and their alloyed Cu2GeSxSe3-x, Cu2ZnGeSxSe4-x nanosheets using pre-synthesized Cu2xSe nanosheets as a template. A mechanism for the formation of Cu2-xSe nanosheets has been studied in detail. In situ oxidation of Cu+ ions to form a CuSe secondary phase facilitates the formation of Cu2-xSe NSs. The obtained ternary and quaternary nanosheets have average lateral size in micrometers and thickness less than 5 nm. This method is general and can be extended to produce other important ternary

  20. Chemistry of alkali cation exchanged faujasite and mesoporous NaX using alkyl halides and phosphates

    NASA Astrophysics Data System (ADS)

    Lee, Min-Hong

    The purpose of this work was to increase the reactivity of Faujasite X (NaX) zeolite toward the reactive decontamination of materials subject to nucleophilic attack by means of zeolite cation optimization and by means of the synthesis of mesoporous Faujasite X. Primary alkyl halides and trialkyl phosphates have been the test materials on which the cation-optimized and mesoporous zeolites have been tested. In the alkali cation optimization work, reactions of methyl iodide and 1-chloropropane with alkali metal cation exchanged Faujasite zeolite X were investigated at room temperature. The reactivity of the framework and the product formation were shown to depend on zeolite framework counter-cation. A quantitative study of zeolite product formation has been carried out, primarily using solid-state NMR spectroscopy. Large alkali cations showed preference toward substitution chemistry. In contrast, alkyl halide exposed LiX and NaX zeolites underwent both substitution and elimination. Subsequently introduced water molecules led to hydrolysis of framework species that was sensitive to framework counter-cation. The mesoporous NaX zeolites work undertakes to test whether an improvement in surface chemical reactivity can be achieved by introducing mesopores into the already reactive nucleophilic microporous NaX zeolite. Incorporation of the polydiallyl dimethyl ammonium chloride (PDADMAC) template and the formation of mesopores in Faujasite X zeolite (NaX) were successful and well-characterized. The mesopores are proposed to have occurred from incorporation of the cationic PDADMAC polymer into the zeolite by compensating zeolite framework charge. Subsequent sodium cation exchange of calcined mesoporous NaX was shown to restore the chemical reactivity characteristic of as-synthesized NaX. Trialkyl organophosphorous compounds underwent substitution reactions. The reactivity of both microporous and mesoporous Faujasite zeolite X and the product formation was shown to depend on

  1. Dielectric phenomena in the cation exchanged/intercalation compounds of MPS[sub 3] materials

    SciTech Connect

    Read, J.A.

    1993-01-01

    The dielectric properties of CdPS[sub 3] and its cation exchanged/intercalation compounds were studied using ac impedance, dc resistance and dc photoconductivity measurements from [minus]130[degrees]C to 400[degrees]C. Cation-vacancy interactions were studied using infrared spectroscopy. Debye relaxation of dipolar motion is observed for the intercalated dipoles in these compounds. Pyridine molecules in the CdPS[sub 3]/Pyridine. H[sup +]/Pyridine compounds give activation energies of 15 to 45 KJ/mole. The activation energy is found to depend on the ratio of pyridine to pyridine [center dot] H[sup +]. CdPS[sub 3] and its cation exchanged/intercalation compounds show activated resistance and capacitance behaviors from 30[degrees]C to 400[degrees]C. The magnitude of the resistance decreases as the activation energy for this behavior increases. The magnitude of the capacitance increases as the activation energy increases. Both behaviors result from holes hopping among vacancy sites in the CdPS[sub 3] lattice. The trends in the activation energies result from vacancy-vacancy interactions that affect the energies of vacancies in the crystal. The wavelength dependent photoconductivity of CdPS[sub 3] shows peaks at 2.94 eV and 3.14 eV. The peaks are interpreted as arising from the excitation of electrons out of two types of vacancy sites in the crystal. The photoconductivity of a de-intercalated CdPS[sub 3]/Pyridine [center dot] H[sup +] crystal gives peaks at 2.95 eV and 3.45 eV. The photoconductivity is found to decrease on cooling and increase with the amount of water absorbed on the surfaces and edges of the crystal. The IR spectra of CdPS[sub 3]/Pyridine [center dot] H[sup +] compounds show consistent splittings in the NH[sup +] band. These splittings are interpreted as arising from the coupling between the fundamental NH[sup +] vibration in pyridine [center dot] H[sup +] and the vibrations of the vacancy site to which it is bound.

  2. [Cation exchanges during the process of Cd(2+) absorption by Alfalfa in aqueous solutions].

    PubMed

    Li, Yue-Peng; Yin, Hua; Ye, Jin-Shao; Peng, Hua; Qin, Hua-Ming; Long, Yan; He, Bao-Yan; Zhang, Na; Tong, Yao; Peng, Su-Fen

    2011-11-01

    A hydroponic experiment was conducted to investigate the cation exchanges during the process of Cd2+ absorption by Alfalfa in aqueous solution. The absorption efficiency of Alfalfa plants with 0-10 mg x L(-1) Cd2+ treatments, changes of Na+, K+, Mg2+, Ca2+ and NH4(+) concentration, and the variation of pH values at different absorption time (0, 1, 2, 4, 8, 12, 24 and 72 h) were studied separately. The multiple linear regressions between Cd2+ absorption and cation variation were analyzed. The results indicated that when Cd2+ concentrations were 0.1, 1, 5, 10 mg x L(-1), the absorption efficiencies of Cd2+ by Alfalfa after 72 h were 85.86%, 52.14%, 15.97% and 7.81%. Cation exchange was involved in the removal of Cd2+ by Alfalfa in aqueous solution. Except for NH4(+), the concentrations of cationic metals Na+, K+, Mg2+ and Ca2+ in aqueous solution increased over time, which increased 11.30% - 61.72%, 21.44% - 98.73%, 24.09% - 8.90% and 37.04% - 191.96%, respectively. Kinetic studies illuminated that the release of Na+, K+, Mg2+ and Ca2+ by Alfalfa in Cd2+ solution with initial concentrations of 0, 0. 1, 1, 5, 10 mg x L(-1) best fitted pseudo-second-order equation,while the NH4(+) release fitted this model when Cd2+ concentrations were 1, 5, 10 mg x L(-1). The gradual decrease of pH during adsorption of Cd2+ by Alfalfa was observed. As the competition ion of Cd2+, H+ might affect the capacity of Alfalfa root system to absorb Cd2+. The ternary linear equation results demonstrated that the content of Cd2+ absorption by Alfalfa strongly related with the release of Ca2+, Mg2+, Na+. And this exchange mainly occurred among Cd2+ and divalent cations. PMID:22295633

  3. Nitrogen removal from wastewater through microbial electrolysis cells and cation exchange membrane

    PubMed Central

    2014-01-01

    Vulnerability of water resources to nutrients led to progressively stricter standards for wastewater effluents. Modification of the conventional procedures to meet the new standards is inevitable. New technologies should give a priority to nitrogen removal. In this paper, ammonium chloride and urine as nitrogen sources were used to investigate the capacity of a microbial electrolysis cell (MEC) configured by cation exchange membrane (CEM) for electrochemical removal of nitrogen over open-and closed-circuit potentials (OCP and CCP) during biodegradation of organic matter. Results obtained from this study indicated that CEM was permeable to both organic and ammonium nitrogen over OCP. Power substantially mediated ammonium migration from anodic wastewater to the cathode, as well. With a urine rich wastewater in the anode, the maximum rate of ammonium intake into the cathode varied from 34.2 to 40.6 mg/L.h over CCP compared to 10.5-14.9 mg/L.h over OCP. Ammonium separation over CCP was directly related to current. For 1.46-2.12 mmol electron produced, 20.5-29.7 mg-N ammonium was removed. Current also increased cathodic pH up to 12, a desirable pH for changing ammonium ion to ammonia gas. Results emphasized the potential for MEC in control of ammonium through ammonium separation and ammonia volatilization provided that membrane characteristic is considered in their development. PMID:24533446

  4. Effects of biofouling on ion transport through cation exchange membranes and microbial fuel cell performance.

    PubMed

    Choi, Mi-Jin; Chae, Kyu-Jung; Ajayi, Folusho F; Kim, Kyoung-Yeol; Yu, Hye-Weon; Kim, Chang-Won; Kim, In S

    2011-01-01

    This study examines the effects of biofouling on the electrochemical properties of cation exchange membranes (CEMs), such as membrane electrical resistance (MER), specific proton conductivity (SC), and ion transport number (t(+)), in addition to on microbial fuel cell (MFC) performance. CEM biofouling using a 15.5 ± 4.6 μm biofilm was found to slightly increase the MER from 15.65 Ω cm(2) (fresh Nafion) to 19.1 Ω cm(2), whereas an increase of almost two times was achieved when the electrolyte was changed from deionized water to an anolyte containing a high cation concentration supporting bacterial growth. The simple physical cleaning of CEMs had little effect on the Coulombic efficiency (CE), whereas replacing a biofouled CEM with new one resulted in considerable increase of up to 59.3%, compared to 45.1% for a biofouled membrane. These results clearly suggest the internal resistance increase of MFC was mainly caused by the sulfonate functional groups of CEM being occupied with cations contained in the anolyte, rather than biofouling itself. PMID:20659795

  5. Bandgap tunable colloidal Cu-based ternary and quaternary chalcogenide nanosheets via partial cation exchange.

    PubMed

    Ramasamy, Parthiban; Kim, Miri; Ra, Hyun-Soo; Kim, Jinkwon; Lee, Jong-Soo

    2016-04-14

    Copper based ternary and quaternary semiconductor nanostructures are of great interest for the fabrication of low cost photovoltaics. Although well-developed syntheses are available for zero dimensional (0D) nanoparticles, colloidal synthesis of two dimensional (2D) nanosheets remains a big challenge. Here we report, for the first time, a simple and reproducible cation exchange approach for 2D colloidal Cu2GeSe3, Cu2ZnGeSe4 and their alloyed Cu2GeSxSe3-x, Cu2ZnGeSxSe4-x nanosheets using pre-synthesized Cu2xSe nanosheets as a template. A mechanism for the formation of Cu2-xSe nanosheets has been studied in detail. In situ oxidation of Cu(+) ions to form a CuSe secondary phase facilitates the formation of Cu2-xSe NSs. The obtained ternary and quaternary nanosheets have average lateral size in micrometers and thickness less than 5 nm. This method is general and can be extended to produce other important ternary semiconductor nanosheets such as CuIn1-xGaxSe2. The optical band gap of these nanosheets is tuned from 1 to 1.48 eV, depending on their composition. PMID:26744188

  6. Effect of ionophores on the rate of intramolecular cation exchange in durosemiquinone ion pairs

    NASA Technical Reports Server (NTRS)

    Eastman, M. P.; Bruno, G. V.; Mcguyer, C. A.; Gutierrez, A. R.; Shannon, J. M.

    1979-01-01

    The effects of the ionophores 15-crown-5 (15C5), 18-crown-6 (18C6), dibenzo-18-crown-6 (DBC) and cryptand 222 (C222) on intramolecular cation exchange in ion pairs of the sodium salt of the durosemiquinone anion in benzene solution are investigated. Electron paramagnetic resonance spectra of the 18C6 and 15C5 complexes with durosemiquinone reduced by contact with a sodium mirror show an alternating line width which indicates that the sodium ion is being exchanged between equivalent sites near the oxygens of the semiquinone with activation energies of 8.7 and 6.0 kcal/mole and Arrhenius preexponential factors of 9 x 10 to the 12th/sec and 10 to the 12th/sec, respectively. Spectra obtained for the DBC complexes show no evidence of exchange, while those of C222 indicate rapid exchange. It is also noted that the hyperfine splitting constants measured do not change over the 50-K temperature interval studied.

  7. Estimating Soil Cation Exchange Capacity from Soil Physical and Chemical Properties

    NASA Astrophysics Data System (ADS)

    Bateni, S. M.; Emamgholizadeh, S.; Shahsavani, D.

    2014-12-01

    The soil Cation Exchange Capacity (CEC) is an important soil characteristic that has many applications in soil science and environmental studies. For example, CEC influences soil fertility by controlling the exchange of ions in the soil. Measurement of CEC is costly and difficult. Consequently, several studies attempted to obtain CEC from readily measurable soil physical and chemical properties such as soil pH, organic matter, soil texture, bulk density, and particle size distribution. These studies have often used multiple regression or artificial neural network models. Regression-based models cannot capture the intricate relationship between CEC and soil physical and chemical attributes and provide inaccurate CEC estimates. Although neural network models perform better than regression methods, they act like a black-box and cannot generate an explicit expression for retrieval of CEC from soil properties. In a departure with regression and neural network models, this study uses Genetic Expression Programming (GEP) and Multivariate Adaptive Regression Splines (MARS) to estimate CEC from easily measurable soil variables such as clay, pH, and OM. CEC estimates from GEP and MARS are compared with measurements at two field sites in Iran. Results show that GEP and MARS can estimate CEC accurately. Also, the MARS model performs slightly better than GEP. Finally, a sensitivity test indicates that organic matter and pH have respectively the least and the most significant impact on CEC.

  8. Morphologically Aligned Cation-Exchange Membranes by a Pulsed Electric Field for Reverse Electrodialysis.

    PubMed

    Lee, Ju-Young; Kim, Jae-Hun; Lee, Ju-Hyuk; Kim, Seok; Moon, Seung-Hyeon

    2015-07-21

    A low-resistance ion-exchange membrane is essential to achieve the high-performance energy conversion or storage systems. The formation methods for low-resistance membranes are various; one of the methods is the ion channel alignment of an ion-exchange membrane under a direct current (DC) electric field. In this study, we suggest a more effective alignment method than the process with the DC electric field. First, an ion-exchange membrane was prepared under a pulsed electric field [alternating current (AC) mode] to enhance the effectiveness of the alignment. The membrane properties and the performance in reverse electrodialysis (RED) were then examined to assess the membrane resistance and ion selectivity. The results show that the membrane electrical resistance (MER) had a lower value of 0.86 Ω cm(2) for the AC membrane than 2.13 Ω cm(2) observed for the DC membrane and 4.30 Ω cm(2) observed for the pristine membrane. Furthermore, RED achieved 1.34 W/m(2) of maximum power density for the AC membrane, whereas that for the DC membrane was found to be 1.14 W/m(2) [a RED stack assembled with CMX, used as a commercial cation-exchange membrane (CEM), showed 1.07 W/m(2)]. Thereby, the novel preparation process for a remarkable low-resistance membrane with high ion selectivity was demonstrated. PMID:26114376

  9. Kinetics and Thermodynamics of Reserpine Adsorption onto Strong Acidic Cationic Exchange Fiber

    PubMed Central

    Guo, Zhanjing; Liu, Xiongmin; Huang, Hongmiao

    2015-01-01

    The kinetics and thermodynamics of the adsorption process of reserpine adsorbed onto the strong acidic cationic exchange fiber (SACEF) were studied by batch adsorption experiments. The adsorption capacity strongly depended on pH values, and the optimum reserpine adsorption onto the SACEF occurred at pH = 5 of reserpine solution. With the increase of temperature and initial concentration, the adsorption capacity increased. The equilibrium was attained within 20 mins. The adsorption process could be better described by the pseudo-second-order model and the Freundlich isotherm model. The calculated activation energy Ea was 4.35 kJ/mol. And the thermodynamic parameters were: 4.97<ΔH<7.44 kJ/mol, -15.29<ΔG<-11.87 kJ/mol and 41.97<ΔS<47.35 J/mol·K. The thermodynamic parameters demonstrated that the adsorption was an endothermic, spontaneous and feasible process of physisorption within the temperature range between 283 K and 323 K and the initial concentration range between 100 mg/L and 300 mg/L. All the results showed that the SACEF had a good adsorption performance for the adsorption of reserpine from alcoholic solution. PMID:26422265

  10. [Preparation of highly hydrophilic strong cation exchangers and their applications in protein analysis].

    PubMed

    Liu, Jizhong; Huang, Yanyan; Yang, Bo; Chang, Jianhua; Liu, Guoquan; Zhao, Rui

    2013-04-01

    Based on the needs of new packing materials for rapid and efficient separation, purification and analysis of biomacromolecules, a novel sulfonic acid-type strong cation exchange resin (SP-G-PGMA SCX resin) was prepared. The porous poly(glycidyl methacrylate) microspheres (PGMA) were selected as the matrix and glucose was used as the hydrophilic modifier to block the hydrophobic domains of PGMA beads. Glucose modification on PGMA beads improved the biocompatibility and reduced the non-specific adsorption so as to increase the recoveries of protein. The PGMA beads possess the porous structure and the relatively high specific surface area, which make the PGMA-based resins good permeability and high loading capacity. The application of such SP-G-PGMA SCX resin for the chromatographic separation of biomacromolecules was explored. Four basic proteins were baseline separated within 6 min with the column size of 100 mm x 4.6 mm. The adsorption capacity of lysozyme on SP-G-PGMA SCX resin was determined as 39.5 g/L. The results make the material promising for the separation and purification of biomacromolecules. PMID:23898627

  11. Independent control of the shape and composition of ionic nanocrystals through sequential cation exchange reactions

    SciTech Connect

    Luther, Joseph Matthew; Zheng, Haimei; Sadtler, Bryce; Alivisatos, A. Paul

    2009-07-06

    Size- and shape-controlled nanocrystal growth is intensely researched for applications including electro-optic, catalytic, and medical devices. Chemical transformations such as cation exchange overcome the limitation of traditional colloidal synthesis, where the nanocrystal shape often reflects the inherent symmetry of the underlying lattice. Here we show that nanocrystals, with established synthetic protocols for high monodispersity, can be templates for independent composition control. Specifically, controlled interconversion between wurtzite CdS, chalcocite Cu2S, and rock salt PbS occurs while preserving the anisotropic dimensions unique to the as-synthesized materials. Sequential exchange reactions between the three sulfide compositions are driven by the disparate solubilites of the metal ion exchange pair in specific coordinating molecules. Starting with CdS, highly anisotropic PbS nanorods are created, which serve as an important material for studying strong 2-dimensional quantum confinement, as well as for optoelectronic applications. Furthermore, interesting nanoheterostructures of CdS|PbS are obtained by precise control over ion insertion and removal.

  12. Analysis of Amadori compounds by high-performance cation exchange chromatography coupled to tandem mass spectrometry.

    PubMed

    Davidek, Tomas; Kraehenbuehl, Karin; Devaud, Stéphanie; Robert, Fabien; Blank, Imre

    2005-01-01

    High-performance cation exchange chromatography coupled to tandem mass spectrometry or electrochemical detection was found to be an efficient tool for analyzing Amadori compounds derived from hexose and pentose sugars. The method allows rapid separation and identification of Amadori compounds, while benefiting from the well-known advantages of mass spectrometry, such as specificity and sensitivity. Glucose- and xylose-derived Amadori compounds of several amino acids, such as glycine, alanine, valine, leucine/isoleucine, methionine, proline, phenylalanine, and glutamic acid, were separated or discriminated using this new method. The method is suitable for the analysis of both model reaction mixtures and food products. Fructosylglutamate was found to be the major Amadori compound in dried tomatoes (approximately 1.5 g/100 g) and fructosylproline in dried apricots (approximately 0.2 g/100 g). Reaction of xylose and glycine at 90 degrees C (pH 6) for 2 h showed rapid formation of xylulosylglycine (approximately 12 mol %, 15 min) followed by slow decrease over time. Analysis of pentose-derived Amadori compounds is shown for the first time, which represents a major breakthrough in studying occurrence, formation, and decomposition of these labile Maillard intermediates. PMID:15623289

  13. Cation exchange resin immobilized bimetallic nickel-iron nanoparticles to facilitate their application in pollutants degradation.

    PubMed

    Ni, Shou-Qing; Yang, Ning

    2014-04-15

    Nanoscale zerovalent iron (nZVI) usually suffers from reduction of reactivity by aggregation, difficulty of assembling, environmental release and health concerns. Furthermore, data are lacking on the effect of cheap nickel on debromination of decabromodiphenyl ether (DBDE) by immobilized nZVI in aqueous system. In this study, strong acid polystyrene cation-exchange resins with particle diameter from 0.4 to 0.6 mm were utilized as matrices to immobilize bimetallic nickel-iron nanoparticles in order to minimize aggregation and environmental leakage risks of nZVI and to enhance their reactivity. Elemental distribution mapping showed that iron particles distributed uniformly on the surface of the resin and nickel particles were dispersed homogeneously into Fe phase. The reaction rate of resin-bound nZVI is about 55% higher than that of dispersed nZVI. The immobilized bimetallic nanoparticles with 9.69% Ni had the highest debromination percent (96%) and reaction rate (0.493 1/h). The existence of Ni significantly improved the debromination rate, due to the surface coverage of catalytic metal on the reductive metal and the formation of a galvanic cell. The environmental dominant congeners, such as BDE 154, 153, 100, 99 and 47, were produced during the process. Outstanding reactive performance, along with magnetic separation assured that resin-bound bimetallic nickel-iron nanoparticles are promising material that can be utilized to remediate a wide variety of pollutants contaminated sites including polybrominated diphenyl ethers. PMID:24559714

  14. Insights into cation exchange selectivity of a natural clinoptilolite by means of dielectric relaxation spectroscopy

    NASA Astrophysics Data System (ADS)

    Rodríguez-Fuentes, Gerardo; Devautour-Vinot, Sabine; Diaby, Sekou; Henn, François

    2011-09-01

    Purified natural clinoptilolite from the Tasajeras deposit, Cuba, and some of its metal exchanged forms are studied, at the dehydrated state, by means of dielectric relaxation spectroscopy (DRS) using two different modus operandi: complex impedance spectroscopy and dielectric dynamic thermal analysis. Data analysis yields the determination of the extra-framework cation (EFC) population into the various possible crystallographic sites of the zeolitic framework as well as of the activation energy characterizing the localized hopping mechanism of EFC. First, it is shown that the DRS responses obtained here match well with the previous reported data, which were previously localized EFCs in positions close to M1 and M2 sites when the clinoptilolite is modified to almost homoionic form. From this outcome, it can be concluded that all EFCs are in the same crystallographic situation regarding solvation or, in other terms, that no steric effect can be taken into account to explain cationic selectivity. Second, based on the assumption that the activation energy for EFC hopping is directly connected to the EFC/framework interaction and on simple thermodynamics consideration, we show this interaction does not govern the EFC exchange reaction. So, it is emphasized that EFC/H2O interaction is the key factor for cation exchange selectivity.

  15. Surface-orientation-dependent distribution of subsurface cation-exchange defects in olivine-phosphate nanocrystals.

    PubMed

    Chung, Sung-Yoon; Choi, Si-Young; Kim, Tae-Hwan; Lee, Seongsu

    2015-01-27

    Atomic-scale exchange between two different cations of similar size in crystalline oxides is one of the major types of point defects when multiple cations in oxygen interstitials are arrayed in an ordered manner. Although a number of studies have been performed on a variety of Li-intercalation olivine phosphates to determine the distribution of exchange defects in bulk, understanding of the thermodynamic stability of the defects in subsurface regions and its dependency on the crystallographic orientation at the surface has remained elusive. Through a combination of small-angle neutron scattering, atomic-scale direct probing with scanning transmission electron microscopy, and theoretical ab initio calculations, we directly demonstrate that the antisite exchange defects are distributed in a highly anisotropic manner near the surfaces of LiFePO4 crystals. Moreover, a substantial amount of cation exchanges between Li and Fe sites is identified as an energetically favorable configuration in some surface regions, showing excellent agreement with the calculation results of negative defect formation energies. The findings in this study provide insight into developing better ways to avoid degradation of lithium mobility through the surface as well as scientifically notable features regarding the distribution of exchange defects in olivine phosphates. PMID:25565086

  16. Adsorption equilibrium and kinetics of monomer-dimer monoclonal antibody mixtures on a cation exchange resin.

    PubMed

    Reck, Jason M; Pabst, Timothy M; Hunter, Alan K; Wang, Xiangyang; Carta, Giorgio

    2015-07-10

    Adsorption equilibrium and kinetics are determined for a monoclonal antibody (mAb) monomer and dimer species, individually and in mixtures, on a macroporous cation exchange resin both under the dilute limit of salt gradient elution chromatography and at high protein loads and low salt based on batch adsorption equilibrium and confocal laser scanning microscopy (CLSM) experiments. In the dilute limit and weak binding conditions, the dimer/monomer selectivity in 10mM phosphate at pH 7 varies between 8.7 and 2.3 decreasing with salt concentration in the range of 170-230mM NaCl. At high protein loads and strong binding conditions (0-60mM NaCl), the selectivity in the same buffer is near unity with no NaCl added, but increases gradually with salt concentration reaching high values between 2 and 15 with 60mM added NaCl. For these conditions, the two-component adsorption kinetics is controlled by pore diffusion and is predicted approximately by a dual shrinking core model using parameters based on single component equilibrium and kinetics measurements. PMID:26028510

  17. Hypercrosslinked strong cation-exchange polymers for selective extraction of serum purine metabolites associated with gout.

    PubMed

    Xu, Yating; Liu, Ju; Zhang, Hongyang; Jiang, Min; Cao, Lingling; Zhang, Min; Sun, Wei; Ruan, Shengli; Hu, Ping

    2016-05-01

    In this study, hypercrosslinked strong cation-exchange polymer resins (HXLPP-SCX) were synthesized and employed as selective sorbents for the solid-phase extraction (SPE) of basic purine metabolites associated with gout. The HXLPP-SCX material was prepared based on hypercrosslinking reactions and sulfonated with concentrated H2SO4. This synthetic procedure is facile and efficient without using highly toxic reagent. The resulting resins were characterized in the form of monodisperse microspheres (mean diameters of 3‒5μm) with narrow pore size (2.1nm) and relatively high specific surface areas (801m(2)/g). The polymers also possess high ion-exchange capacity (IEC, 2.22mmol/g) and good adsorption and selectivity performances for basic compounds. The resins used as SPE sorbents permit the selective enrichment of three pivotal purine metabolites (hypoxanthine, xanthine and inosine) in human serum followed by HPLC analysis. Method validation including linearity range, sensitivity, accuracy and reproducibility were evaluated. This method was exemplarily applied in the analysis of serum purines in gout patients and healthy controls. The present results demonstrate a promising potential of this HXLPP-SCX material for the clinical sample pretreatment. PMID:26946024

  18. Effects of experimental conditions on extraction yield of extracellular polymeric substances by cation exchange resin.

    PubMed

    Cho, Jinwoo; Hermanowicz, Slawomir W; Hur, Jin

    2012-01-01

    Effects of experimental conditions on the yield of extracellular polymeric substances (EPSs) extraction by cation exchange resin (CER) were investigated using activated sludge flocs. The experimental variables included resin dose, extraction time, sample dilution, and storage time. An empirical model was proposed to describe the kinetics of extraction process. The extraction yield increases with the extraction time and CER dose until it reached the maximum amount of EPS extraction. The maximum yield of EPS was affected as well by the sample dilution, exhibiting a decreasing trend with increasing dilution factor. It was also found that the amount of EPS extracted from a raw sample depends on the storage time. Once EPS was extracted from the sample, however, the EPS keeps its original quantity under storage at 4°C. Based on the model, the maximum amount of EPS extraction and yield rate could be estimated for different conditions. Comparing the model parameters allows one to quantitatively compare the extraction efficiencies under various extracting conditions. Based on the results, we recommend the original sample should be diluted with the volume ratio of above 1:2 and a raw sample should be treated quickly to prevent the reduction of sample homogeneity and original integrity. PMID:22919352

  19. Characterization of perfluorinated cation-exchange membranes MF-4SC surface modified with halloysite nanotubes

    NASA Astrophysics Data System (ADS)

    Filippov, A.; Afonin, D.; Kononenko, N.; Shkirskaya, S.

    2015-10-01

    The electrical conductivity and diffusion permeability through perfluorinated cation-exchange membranes MF-4SC (Russian analog of the Nafion-type membrane), whose surface is modified by nanotubes of halloysite using short exposures of low temperature microwave plasma, are theoretically investigated using the Nernst-Planck approach. The method of quantitative evaluation of physicochemical parameters (individual and averaged diffusion coefficients and averaged distribution coefficients of ion pairs in the membrane) of the systems `electrolyte solution - bi-layer ion-exchange membrane - water/electrolyte solution', which was proposed by us earlier, is further developed. The aforementioned parameters of modified MF-4SC/halloysite membranes were found using the least squares method. For this purpose we used electrical conductivity as well as diffusion permeability data experimentally obtained for NaCl and HCl solutions of different concentration. A new model of bi-layer membrane system can be used for refining the calculated results by taking into account the difference between co- and counter-ion diffusivities inside the membrane layers. We showed that grafting the layer of halloysite nanotubes onto the membrane surface noticeably affects the exchange capacity as well as the structural and transport characteristics of the original perfluorinated membrane. In particular, such a membrane may show weak asymmetry of diffusion permeability when its position inside a measuring cell is changed. Hybrid MF-4SC/halloysite membranes can thus be productively used in fuel cells and catalysis.

  20. Solvent modulation strategy for superior antibody monomer/aggregate separation in cation exchange chromatography.

    PubMed

    Kluters, Simon; Frech, Christian; von Hirschheydt, Thomas; Schaubmar, Andreas; Neumann, Sebastian

    2015-12-01

    Cation exchange chromatography (CEX) is an integral part of many downstream processes for monoclonal antibodies (mAbs). However, in some cases CEX methods with standard mobile phase conditions do not lead to a sufficient removal of soluble antibody aggregates. The addition of neutral polymers such as polyethylene glycol (PEG) to the mobile phase can improve the separation of proteins in IEC remarkably. The applicability of this solvent modulation technique is limited by protein precipitation at higher PEG concentrations. To overcome this limitation solubility enhancers like polyols and amino acids can be added to the mobile phase. These additives are known to inhibit PEG-induced protein precipitation in solution. This new solvent modulation strategy was tested with three different mAbs on two different CEX resins in the presence of PEG in combination with various solubility enhancers. In order to assess the general applicability of this method, mAbs were selected that show major differences with respect to their sensitivity to PEG-induced precipitation and monomer/aggregate resolution performance that is achieved by CEX under standard conditions. For all three mAbs precipitation could be prevented without elimination of the positive PEG-effect. The addition of solubility enhancers gives access to improved separation at elevated PEG concentrations and high protein loadings without running into precipitation issues. Our data indicate that this method is generically applicable and leads to a superior antibody monomer/aggregate separation. PMID:26520020

  1. Composite membranes prepared from cation exchange membranes and polyaniline and their transport properties in electrodialysis

    SciTech Connect

    Sata, Tshikatsu; Ishii, Yuuko; Kawamura, Kohei; Matsusaki, Koji

    1999-02-01

    A cation exchange membrane was modified with polyaniline by polymerizing aniline with ammonium peroxodisulfate on the membrane surfaces, producing a membrane with polyaniline layers on both surfaces or a membrane with a single polyaniline layer on the surface. The modified membranes, composite membranes, showed sodium ion permselectivity in electrodialysis compared with divalent cations at an optimum polymerization time. The electronic conductivity of dry membranes showed a maximum (ca. 5 {times} 10{sup {minus}3} S/cm) at the same polymerization time as the time to attain a maximum value of the sodium ion permselectivity. Because emeraldine-based polyaniline is conductive and has a cationic charge, the sodium ion permselectivity is based on the difference in the electrostatic repulsion forces of the cationic charge on the membrane surface of a desalting side to divalent cations and sodium ions. In fact, the selective permeation of sodium ions appeared only when the layer faced the desalting side of the membrane, and was affected by dissociation of polyaniline. Further oxidized polyaniline, pernigraniline-based polyaniline, did not affect the permselectivity between cations, and the diffusion coefficient of neutral molecules, urea, increased with increasing polymerization time. Sodium ion permselectivity was maintained with repeated electrodialysis.

  2. Fluorescent metal ion chemosensors via cation exchange reactions of complexes, quantum dots, and metal-organic frameworks.

    PubMed

    Cheng, Jinghui; Zhou, Xiangge; Xiang, Haifeng

    2015-11-01

    Due to their wide range of applications and biological significance, fluorescent sensors have been an active research area in the past few years. In the present review, recent research developments on fluorescent chemosensors that detect metal ions via cation exchange reactions (transmetalation, metal displacement, or metal exchange reactions) of complexes, quantum dots, and metal-organic frameworks are described. These complex-based chemosensors might have a much better selectivity than the corresponding free ligands/receptors because of the shielding function of the filled-in metal ions. Moreover, not only the chemical structure of the ligands/receptors but also the identity of the central metal ions have a tremendous impact on the sensing performances. Therefore, sensing via cation exchange reactions potentially provides a new, simple, and powerful way to design fluorescent chemosensors. PMID:26375420

  3. Effect of temperature on REE and TPE sorption by sulfonated cation exchangers from HNO{sub 3} solutions

    SciTech Connect

    Chuveleva, E.A.; Kharitonov, O.V.; Firsova, L.A.

    1995-05-01

    Numerical and experimental data are presented for sorption from HNO{sub 3} solutions on KU-2 sulfonated cation exchanger as a function of temperature. The capacity for Eu at 70{degrees}C for solutions with [H{sup +}] > 1.0 M in the range [Eu] = 0.023-0.0428 M increases by 20-30%. The width of the sorption front significantly decreases at elevated temperature. The calculations are consistent with the observed experimental sorption process.

  4. Cesium migration in Hanford sediment: a multisite cation exchange model based on laboratory transport experiments

    NASA Astrophysics Data System (ADS)

    Steefel, Carl I.; Carroll, Susan; Zhao, Pihong; Roberts, Sarah

    2003-12-01

    Cs + transport experiments carried out in columns packed with uncontaminated Hanford formation sediment from the SX tank farm provide strong support for the use of a multisite, multicomponent cation exchange model to describe Cs + migration in the Hanford vadose zone. The experimental results indicate a strong dependence of the effective Cs +Kd on the concentrations of other cations, including Na + that is present at high to extremely high concentrations in fluids leaking from the Hanford SX tanks. A strong dependence of the Cs +Kd on the aqueous Cs + concentration is also apparent, with retardation of Cs + increasing from a value of 41 at a Cs + concentration of 10 -4 M in the feed solution to as much as 282 at a Cs + concentration of 5×10 -7 M, all in a background of 1 M NaNO 3. The total cation exchange capacity (CEC) of the Hanford sediment was determined using 22Na isotopic equilibrium exchange in a flow-through column experiment. The value for the CEC of 120 μeq/g determined with this method is compatible with a value of 121.9 μeq/g determined by multi-cation elution. While two distinct exchange sites were proposed by Zachara et al. [Geochim. Cosmochim. Acta 66 (2002) 193] based on binary batch exchange experiments, a third site is proposed in this study to improve the fit of the Cs +-Na + and Cs +-Ca + exchange data and to capture self-sharpened Cs + breakthrough curves at low concentrations of Cs +. Two of the proposed exchange sites represent frayed edge sites (FES) on weathered micas and constitute 0.02% and 0.22% of the total CEC. Both of the FES show a very strong selectivity for Cs + over Na + ( KNa-Cs=10 7.22 and 10 4.93, respectively). The third site, accounting for over 99% of the total CEC, is associated with planar sites on expansible clays and shows a smaller Na +-Cs + selectivity coefficient of 10 1.99. Parameters derived from a fit of binary batch experiments alone tend to under predict Cs + retardation in the column experiments. The

  5. Cesium migration in Hanford sediment: a multisite cation exchange model based on laboratory transport experiments.

    PubMed

    Steefel, Carl I; Carroll, Susan; Zhao, Pihong; Roberts, Sarah

    2003-12-01

    Cs+ transport experiments carried out in columns packed with uncontaminated Hanford formation sediment from the SX tank farm provide strong support for the use of a multisite, multicomponent cation exchange model to describe Cs+ migration in the Hanford vadose zone. The experimental results indicate a strong dependence of the effective Cs+ Kd on the concentrations of other cations, including Na+ that is present at high to extremely high concentrations in fluids leaking from the Hanford SX tanks. A strong dependence of the Cs+ Kd on the aqueous Cs+ concentration is also apparent, with retardation of Cs+ increasing from a value of 41 at a Cs+ concentration of 10(-4) M in the feed solution to as much as 282 at a Cs+ concentration of 5x10(-7) M, all in a background of 1 M NaNO3. The total cation exchange capacity (CEC) of the Hanford sediment was determined using 22Na isotopic equilibrium exchange in a flow-through column experiment. The value for the CEC of 120 microeq/g determined with this method is compatible with a value of 121.9 microeq/g determined by multi-cation elution. While two distinct exchange sites were proposed by Zachara et al. [Geochim. Cosmochim. Acta 66 (2002) 193] based on binary batch exchange experiments, a third site is proposed in this study to improve the fit of the Cs+-Na+ and Cs+-Ca+ exchange data and to capture self-sharpened Cs+ breakthrough curves at low concentrations of Cs+. Two of the proposed exchange sites represent frayed edge sites (FES) on weathered micas and constitute 0.02% and 0.22% of the total CEC. Both of the FES show a very strong selectivity for Cs+ over Na+ (K(Na-Cs)=10(7.22) and 10(4.93), respectively). The third site, accounting for over 99% of the total CEC, is associated with planar sites on expansible clays and shows a smaller Na+-Cs+ selectivity coefficient of 10(1.99). Parameters derived from a fit of binary batch experiments alone tend to under predict Cs+ retardation in the column experiments. The transport

  6. Action of colloidal silica films on different nano-composites

    NASA Astrophysics Data System (ADS)

    Abdalla, S.; Al-Marzouki, F.; Obaid, A.; Gamal, S.

    Nano-composite films have been the subject of extensive work to develop the energy-storage efficiency of electrostatic capacitors. Factors such as polymer purity, nano-particles size, and film morphology drastically affect the electrostatic efficiency of the dielectric material that form an insulating film between conductive electrodes of a capacitor. This in turn affects the energy storage performance of the capacitor. In the present work, we have studied the dielectric properties of 4 high pure amorphous polymer films: polymethylmethacrylate (PMMA), polystyrene, polyimide and poly-4-vinylpyridine. Comparison between the dielectric properties of these polymers has revealed that the higher break down performance is a character of polyimide PI and PMMA. Also, our experimental data shows that adding colloidal silica to PMMA and PI leads to a net decrease in the dielectric properties compared to the pure polymer.

  7. First study of nano-composite scintillators under alpha irradiation

    SciTech Connect

    Letant, S; Wang, T

    2005-06-01

    We demonstrate that nano-composite materials based on semiconductor quantum dots have great potential for radiation detection via scintillation. While quantum dots and laser dyes both emit in the visible range at room temperature, the Stokes shift of the dyes is significantly larger. The scintillation output of both systems was studied under alpha irradiation and interpreted using a combination of energy-loss and photon transport Monte Carlo simulation models. The comparison of the two systems, which allows the quantification of the role played by the Stokes shift in the scintillation output, opens up exciting possibilities for a new class of scintillators that would take advantage of the limitless assembly of nano-crystals in large, transparent, and sturdy matrices.

  8. Utilization of cation exchange resins for the isolation and separation of transplutonium elements from others in aqueous and non aqueous-alcohol solutions of hydrochloric and nitric acids

    SciTech Connect

    Guseva, L.I.; Tikhomirova, G.S.

    1985-07-01

    The authors study the sorption of several transplutonium and fission elements on cation exchange resins in relation to the acid concentration and content of alcohol in solution. They observe a significant increase in sorption of the TPE on the cation exchanges from nitric acid solutions containing more than 50% of alcohol. On the basis of the experimental results they determine the optimum conditions for the concentration of TPE on cation exchangers with their subsequent separation from certain fission and other elements by means of hydrochloric acid and nitric acid solutions.

  9. Probing the Complementarity of FAIMS and Strong Cation Exchange Chromatography in Shotgun Proteomics

    NASA Astrophysics Data System (ADS)

    Creese, Andrew J.; Shimwell, Neil J.; Larkins, Katherine P. B.; Heath, John K.; Cooper, Helen J.

    2013-03-01

    High field asymmetric waveform ion mobility spectrometry (FAIMS), also known as differential ion mobility spectrometry, coupled with liquid chromatography tandem mass spectrometry (LC-MS/MS) offers benefits for the analysis of complex proteomics samples. Advantages include increased dynamic range, increased signal-to-noise, and reduced interference from ions of similar m/ z. FAIMS also separates isomers and positional variants. An alternative, and more established, method of reducing sample complexity is prefractionation by use of strong cation exchange chromatography. Here, we have compared SCX-LC-MS/MS with LC-FAIMS-MS/MS for the identification of peptides and proteins from whole cell lysates from the breast carcinoma SUM52 cell line. Two FAIMS approaches are considered: (1) multiple compensation voltages within a single LC-MS/MS analysis (internal stepping) and (2) repeat LC-MS/MS analyses at different and fixed compensation voltages (external stepping). We also consider the consequence of the fragmentation method (electron transfer dissociation or collision-induced dissociation) on the workflow performance. The external stepping approach resulted in a greater number of protein and peptide identifications than the internal stepping approach for both ETD and CID MS/MS, suggesting that this should be the method of choice for FAIMS proteomics experiments. The overlap in protein identifications from the SCX method and the external FAIMS method was ~25 % for both ETD and CID, and for peptides was less than 20 %. The lack of overlap between FAIMS and SCX highlights the complementarity of the two techniques. Charge state analysis of the peptide assignments showed that the FAIMS approach identified a much greater proportion of triply-charged ions.

  10. Sn Cation Valency Dependence in Cation Exchange Reactions Involving Cu2-xSe Nanocrystals

    PubMed Central

    2014-01-01

    We studied cation exchange reactions in colloidal Cu2-xSe nanocrystals (NCs) involving the replacement of Cu+ cations with either Sn2+ or Sn4+ cations. This is a model system in several aspects: first, the +2 and +4 oxidation states for tin are relatively stable; in addition, the phase of the Cu2-xSe NCs remains cubic regardless of the degree of copper deficiency (that is, “x”) in the NC lattice. Also, Sn4+ ions are comparable in size to the Cu+ ions, while Sn2+ ones are much larger. We show here that the valency of the entering Sn ions dictates the structure and composition not only of the final products but also of the intermediate steps of the exchange. When Sn4+ cations are used, alloyed Cu2–4ySnySe NCs (with y ≤ 0.33) are formed as intermediates, with almost no distortion of the anion framework, apart from a small contraction. In this exchange reaction the final stoichiometry of the NCs cannot go beyond Cu0.66Sn0.33Se (that is Cu2SnSe3), as any further replacement of Cu+ cations with Sn4+ cations would require a drastic reorganization of the anion framework, which is not possible at the reaction conditions of the experiments. When instead Sn2+ cations are employed, SnSe NCs are formed, mostly in the orthorhombic phase, with significant, albeit not drastic, distortion of the anion framework. Intermediate steps in this exchange reaction are represented by Janus-type Cu2-xSe/SnSe heterostructures, with no Cu–Sn–Se alloys. PMID:25340627

  11. A new cation-exchange method for accurate field speciation of hexavalent chromium

    USGS Publications Warehouse

    Ball, J.W.; McCleskey, R.B.

    2003-01-01

    A new method for field speciation of Cr(VI) has been developed to meet present stringent regulatory standards and to overcome the limitations of existing methods. The method consists of passing a water sample through strong acid cation-exchange resin at the field site, where Cr(III) is retained while Cr(VI) passes into the effluent and is preserved for later determination. The method is simple, rapid, portable, and accurate, and makes use of readily available, inexpensive materials. Cr(VI) concentrations are determined later in the laboratory using any elemental analysis instrument sufficiently sensitive to measure the Cr(VI) concentrations of interest. The new method allows measurement of Cr(VI) concentrations as low as 0.05 ??g 1-1, storage of samples for at least several weeks prior to analysis, and use of readily available analytical instrumentation. Cr(VI) can be separated from Cr(III) between pH 2 and 11 at Cr(III)/Cr(VI) concentration ratios as high as 1000. The new method has demonstrated excellent comparability with two commonly used methods, the Hach Company direct colorimetric method and USEPA method 218.6. The new method is superior to the Hach direct colorimetric method owing to its relative sensitivity and simplicity. The new method is superior to USEPA method 218.6 in the presence of Fe(II) concentrations up to 1 mg 1-1 and Fe(III) concentrations up to 10 mg 1-1. Time stability of preserved samples is a significant advantage over the 24-h time constraint specified for USEPA method 218.6.

  12. Separation of proteins by cation-exchange sequential injection chromatography using a polymeric monolithic column.

    PubMed

    Masini, Jorge Cesar

    2016-02-01

    Since sequential injection chromatography (SIC) emerged in 2003, it has been used for separation of small molecules in diverse samples, but separations of high molar mass compounds such as proteins have not yet been described. In the present work a poly(glycidyl methacrylate-co-ethylene dimethacrylate) (GMA-co-EDMA) monolithic column was prepared by free radical polymerization inside a 2.1-mm-i.d. activated fused silica-lined stainless steel tubing and modified with iminodiacetic acid (IDA). The column was prepared from a mixture of 24% GMA, 16% EDMA, 20% cyclohexanol, and 40% 1-dodecanol (all% as w/w) containing 1% of azobisisobutyronitrile (AIBN) (in relation to monomers). Polymerization was done at 60 °C for 24 h. The polymer was modified with 1.0 M IDA (in 2 M Na2CO3, pH 10.5) at 80 °C for 16 h. Separation of myoglobin, ribonuclease A, cytochrome C, and lysozyme was achieved at pH 7.0 (20 mM KH2PO4/K2HPO4) using a salt gradient (NaCl). Myoglobin was not retained, and the other proteins were separated by a gradient of NaCl created inside the holding coil (4 m of 0.8-mm-i.d. PTFE tubing) by sequential aspiration of 750 and 700 μL of 0.2 and 0.1 M NaCl, respectively. As the flow was reversed toward the column (5 μL s(-1)) the interdispersion of these solutions created a reproducible gradient which separated the proteins in 10 min, with the following order of retention: ribonuclease A < cytochrome C < lysozyme. The elution order was consistent with a cation-exchange mechanism as the retention increased with the isoelectric points. PMID:26677024

  13. Cation exchange capacity of loess and overlying soil in the non-carbonate loess sections, North-Western Croatia

    NASA Astrophysics Data System (ADS)

    Tomašić, Nenad; Kampić, Štefica; Cindrić, Iva Juranović; Pikelj, Kristina; Lučić, Mavro; Mavrić, Danijela; Vučetić, Tajana

    2013-12-01

    The adsorption properties in terms of cation exchange capacity and their relation to the soil and sediment constituents (clay minerals, Fe-, Mn-, and Al-oxyhydroxides, organic matter) were investigated in loess, soil-loess transition zone, and soil at four loess-soil sections in North-Western Croatia. Cation exchange capacity of the bulk samples, the samples after oxalate extraction of Fe, Mn and Al, and after removal of organic matter, as well as of the separated clay fraction, was determined using copper ethylenediamine. Cation exchange capacity (pH˜7) of the bulk samples ranges from 5 to 12 cmol c /kg in soil, from 7 to 15 cmol c /kg in the soil-loess transition zone, and from 12 to 20 cmol c /kg in loess. Generally, CEC values increase with depth. Oxalate extraction of Fe, Mn, and Al, and removal of organic matter cause a CEC decrease of 3-38% and 8-55%, respectively, proving a considerable influence of these constituents to the bulk CEC values. In the separated clay fraction (<2 μm) CEC values are up to several times higher relative to those in the bulk samples. The measured CEC values of the bulk samples generally correspond to the clay mineral content identified. Also, a slight increase in muscovite/illite content with depth and the vermiculite occurrence in the loess horizon are concomitant with the CEC increase in deeper horizons, irrespective of the sample pretreatment.

  14. Cation exchange capacity of loess and overlying soil in the non-carbonate loess sections, North-Western Croatia

    NASA Astrophysics Data System (ADS)

    Tomašić, Nenad; Kampić, Štefica; Cindrić, Iva; Pikelj, Kristina; Lučić, Mavro; Mavrić, Danijela; Vučetić, Tajana

    2013-12-01

    The adsorption properties in terms of cation exchange capacity and their relation to the soil and sediment constituents (clay minerals, Fe-, Mn-, and Al-oxyhydroxides, organic matter) were investigated in loess, soil-loess transition zone, and soil at four loess-soil sections in North-Western Croatia. Cation exchange capacity of the bulk samples, the samples after oxalate extraction of Fe, Mn and Al, and after removal of organic matter, as well as of the separated clay fraction, was determined using copper ethylenediamine. Cation exchange capacity (pH˜7) of the bulk samples ranges from 5 to 12 cmolc/kg in soil, from 7 to 15 cmolc/kg in the soil-loess transition zone, and from 12 to 20 cmolc/kg in loess. Generally, CEC values increase with depth. Oxalate extraction of Fe, Mn, and Al, and removal of organic matter cause a CEC decrease of 3-38% and 8-55%, respectively, proving a considerable influence of these constituents to the bulk CEC values. In the separated clay fraction (<2 μm) CEC values are up to several times higher relative to those in the bulk samples. The measured CEC values of the bulk samples generally correspond to the clay mineral content identified. Also, a slight increase in muscovite/illite content with depth and the vermiculite occurrence in the loess horizon are concomitant with the CEC increase in deeper horizons, irrespective of the sample pretreatment.

  15. Retardation of ammonium and potassium transport through a contaminated sand and gravel aquifer: The Role of cation exchange

    USGS Publications Warehouse

    Ceazan, M.L.; Thurman, E.M.; Smith, R.L.

    1989-01-01

    The role of cation exchange in the retardation of ammonium (NH4+) and potassium (K+) transport in a shallow sand and gravel aquifer was evaluated by use of observed distributions of NH4+ and K+ within a plume of sewage-contaminated groundwater, small-scale tracer injection tests, and batch sorption experiments on aquifer material. Both NH4+ and K+ were transported ???2 km in the 4-km-long contaminant plume (retardation factor, Rf = 2.0). Sediments from the NH4+-containing zone of the plume contained significant quantities of KCl-extractable NH4+ (extraction distribution coefficient, Kd,extr = 0.59-0.87 mL/g of dry sediment), and when added to uncontaminated sediments, NH4+ sorption followed a linear isotherm. Small-scale tracer tests demonstrated that NH4+ and K+ were retarded (Rf =3.5) relative to a nonreactive tracer (Br-). Sorption of dissolved NH4+ was accompanied by concomitant release of calcium (Ca2+), magnesium (Mg2+), and sodium (Na+) from aquifer sediments, suggesting involvement of cation exchange. In contrast, nitrate (NO3-) was not retarded and cleanly separated from NH4+ and K+ in the small-scale tracer tests. This study demonstrates that transport of NH4+ and K+ through a sand and gravel aquifer can be markedly affected by cation-exchange processes even at a clay content less than 0.1%.

  16. Stress development in particulate, nano-composite and polymeric coatings

    NASA Astrophysics Data System (ADS)

    Jindal, Karan

    2009-12-01

    The main goal of this research is to study the stress, structural and mechanical property development during the drying of particulate coatings, nano-composite coatings and VOC compliant refinish clearcoats. The results obtained during this research establish the mechanism for the stress development during drying in various coating systems. Coating stress was measured using a controlled environment stress apparatus based on cantilever deflection principle. The stress evolution in alumina coatings made of 0.4 mum size alumina particles was studied and the effect of a lateral drying was investigated. The stress does not develop until the later stages of drying. A peak stress was observed during drying and the peak stress originates due to the formation of pendular rings between the particles. Silica nanocomposite coatings were fabricated from suspension of nano sized silicon dioxide particles (20 nm) and polyvinyl alcohol (PVA) polymer. The stress in silica nano-composite goes through maximum as the amount of polymer in the coating increases. The highest final stress was found to be ˜ 110MPa at a PVA content of 60 wt%. Observations from SEM, nitrogen gas adsorption, camera imaging, and nano-indentation were also studied to correlate the coatings properties during drying to measured stress. A model VOC compliant two component (2K) acrylic-polyol refinish clearcoat was prepared to study the effects of a new additive on drying, curing, rheology and stress development at room temperature. Most of the drying of the low VOC coatings occurred before appreciable (20%) crosslinking. Tensile stress developed in the same timeframe as drying and then relaxed over a longer time scale. Model low VOC coatings prepared with the additive had higher peak stresses than those without the additive. In addition, rheological data showed that the additive resulted in greater viscosity buildup during drying.

  17. Preparation of poly(glycidylmethacrylate-divinylbenzene) weak acid cation exchange stationary phases with succinic anhydride, phthalic anhydride, and maleic anhydride for ion chromatography.

    PubMed

    Liu, Junwei; Wang, Yong; Wu, Shuchao; Zhang, Peimin; Zhu, Yan

    2016-08-01

    In this work, poly(glycidylmethacrylate-divinylbenzene) microspheres were prepared and applied for the preparation of weak acid cation exchange stationary phases. Succinic anhydride, phthalic anhydride, and maleic anhydride were selected as carboxylation reagents to prepare three weak acid cation exchangers by direct chemical derivatization reaction without solvent or catalyst. The diameters and dispersity of the microspheres were characterized by scanning electron microscopy; the amount of accessible epoxy groups and mechanical stability were also measured. The weak acid cation exchangers were characterized by Fourier transform infrared spectroscopy; the content of carboxyl groups was measured by traditional acid base titration method. The chromatographic properties were characterized and compared by separating alkali, alkaline earth metal ions and ammonium and polar amines. The separation properties enhanced in the order of succinic anhydride, phthalic anhydride, and maleic anhydride modified poly(glycidylmethacrylate-divinylbenzene) cation exchangers. PMID:27288092

  18. Use of zirconium(IV) arsenophosphate columns for cation exchange separation of metal ions interfering in the spectrophotometric determination of uranium with sodium diethyl dithiocarbamate

    SciTech Connect

    Varshney, K.G.; Agrawal, S.; Anwar, S.; Varshney, K.

    1985-01-01

    A simple cation exchange method has been developed for the quantitative separation of uranium from some metal ions which generally interfere in its spectrophotometric determination using sodium diethyl dithiocarbamate as a reagent. The method requires only a single bed operation and enables a satisfactory (Error + or - separation of uranium (UO/sub 2/ (II)) up to 1080 ..mu..g from ten metal ions on a 2 g column of zirconium (IV) arsenophosphate cation exchanger in H(I) form.

  19. Cation-cation interactions and cation exchange in a series of isostructural framework uranyl tungstates

    NASA Astrophysics Data System (ADS)

    Balboni, Enrica; Burns, Peter C.

    2014-05-01

    The isotypical compounds (UO2)3(WO6)(H2O)5 (1), Ag(UO2)3(WO6)(OH)(H2O)3 (2), K(UO2)3(WO6)OH(H2O)4 (3), Rb(UO2)3(WO6)(OH)(H2O)3.5 (4), and Cs(UO2)3(WO6)OH(H2O)3 (5) were synthesized, characterized, and their structures determined. Each crystallizes in space group Cc. (1): a=12.979 (3), b=10.238 (2), c=11.302 (2), β=102.044 (2); (2): a=13.148 (2), b=9.520 (1), c=11.083 (2), β=101.568 (2); (3): a=13.111 (8), b=9.930 (6), c=11.242 (7), β=101.024 (7); (4): a=12.940 (2), b=10.231 (2), c=11.259(2), β=102.205 (2); (5): a=12.983 (3), b=10.191 (3), c=11.263 (4), β=101.661 (4). Compounds 1-5 are a framework of uranyl and tungsten polyhedra containing cation-cation interactions. The framework has three symmetrically distinct U(VI) cations, one tungsten, sixteen to eighteen oxygen atoms, and in 2-5, one monovalent cation. Each atom occupies a general position. Each U(VI) cation is present as a typical (UO2)2+ uranyl ion in an overall pentagonal bipyramidal coordination environment. Each pentagonal bipyramid shares two equatorial edges with two other pentagonal bipyramids, forming a trimer. Trimers are connected into chains by edge-sharing with WO6 octahedra. Chains are linked through cation-cation interactions between two symmetrically independent uranyl ions. This yields a remarkably complex system of intersecting channels that extend along [0 0 1] and [-1 1 0]. The cation exchange properties of 2 and 3 were characterized at room temperature and at 140 °C.

  20. Synthesis of Mesostructured Copper Sulfide by Cation Exchange and Liquid Crystal Templating

    SciTech Connect

    Lubeck, C R; Doyle, F M; Gash, A E; Satcher, J H; Han, T Y

    2005-08-01

    describe for the first time, the successful synthesis of highly ordered, mesostructured Cu{sub x}S, by combining the templating of the supramolecular assemblies of non-ionic amphiphilic polymer method with the cation exchange method to transform mesostructured cadmium sulfide (CdS) into mesostructured copper sulfides (CuS, Cu{sub 2}S).

  1. Chemically modified polypyrrole

    SciTech Connect

    Inagaki, T.; Skotheim, T.A.; Lee, H.S.; Okamoto, Y.; Samuelson, L.; Tripathy, S.

    1988-01-01

    Polypyrrole (PPy) films have been systematically modified with electroactive groups in the ..beta..-position to design electrode materials with specific electrochemical and surface active properties. Electrochemical copolymerization of pyrrole and 3-(6-ferrocenyl,6-hydroxyhexyl)pyrrole (P-6-Fc) yields a ferrocene functionalized polypyrrole with a controlled amount to ferrocene functionalization. And also, copolymers of pyrrole and 3-(4-(2,5- dimethoxyphenyl)butyl)pyrrole (P-MP) can be made by electrochemical polymerization and converted to the copolymers containing pH dependent electroactive hydroquinone moieties. Derivatized pyrroles have also been incorporated into Langmuir-Blodgett film structures. The surface pressure-area isotherms of 3-(13-ferrocenyl,13-hydroxytridecy)pyrrole (P-13-Fc) and the mixed monolayer of P-13-Fc and 3-n-hexadecylpyrrole (HDP) are shown. 17 refs., 4 figs.

  2. Lightweight Aluminum/Nano composites for Automotive Drive Train Applications

    SciTech Connect

    Chelluri, Bhanumathi; Knoth, Edward A.; Schumaker, Edward J.

    2012-12-14

    During Phase I, we successfully processed air atomized aluminum powders via Dynamic Magnetic Compaction (DMC) pressing and subsequent sintering to produce parts with properties similar to wrought aluminum. We have also showed for the first time that aluminum powders can be processed without lubes via press and sintering to 100 % density. This will preclude a delube cycle in sintering and promote environmentally friendly P/M processing. Processing aluminum powders via press and sintering with minimum shrinkage will enable net shape fabrication. Aluminum powders processed via a conventional powder metallurgy process produce too large a shrinkage. Because of this, sinter parts have to be machined into specific net shape. This results in increased scrap and cost. Fully sintered aluminum alloy under this Phase I project has shown good particle-to-particle bonding and mechanical properties. We have also shown the feasibility of preparing nano composite powders and processing via pressing and sintering. This was accomplished by dispersing nano silicon carbide (SiC) powders into aluminum matrix comprising micron-sized powders (<100 microns) using a proprietary process. These composite powders of Al with nano SiC were processed using DMC press and sinter process to sinter density of 85-90%. The process optimization along with sintering needs to be carried out to produce full density composites.

  3. PREFACE: International Conference on Structural Nano Composites (NANOSTRUC 2012)

    NASA Astrophysics Data System (ADS)

    Njuguna, James

    2012-09-01

    Dear Colleagues It is a great pleasure to welcome you to NanoStruc2012 at Cranfield University. The purpose of the 2012 International Conference on Structural Nano Composites (NanoStruc2012) is to promote activities in various areas of materials and structures by providing a forum for exchange of ideas, presentation of technical achievements and discussion of future directions. NanoStruc brings together an international community of experts to discuss the state-of-the-art, new research results, perspectives of future developments, and innovative applications relevant to structural materials, engineering structures, nanocomposites, modelling and simulations, and their related application areas. The conference is split in 7 panel sessions, Metallic Nanocomposites and Coatings, Silica based Nanocomposites, safty of Nanomaterials, Carboin based Nanocomposites, Multscale Modelling, Bio materials and Application of Nanomaterials. All accepted Papers will be published in the IOP Conference Series: Materials Science and Engineering (MSE), and included in the NanoStruc online digital library. The abstracts will be indexed in Scopus, Compedex, Inspec, INIS (International Nuclear Information System), Chemical Abstracts, NASA Astrophysics Data System and Polymer Library. Before ending this message, I would like to acknowledge the hard work, professional skills and efficiency of the team which ensured the general organisation. As a conclusion, I would like to Welcome you to the Nanostruc2012 and wish you a stimulating Conference and a wonderful time. On behalf of the scientific committee, Signature James Njuguna Conference Chair The PDF of this preface also contains committee listings and associates logos.

  4. Anion- or Cation-Exchange Membranes for NaBH4/H2O2 Fuel Cells?

    PubMed

    Sljukić, Biljana; Morais, Ana L; Santos, Diogo M F; Sequeira, César A C

    2012-01-01

    Direct borohydride fuel cells (DBFC), which operate on sodium borohydride (NaBH4) as the fuel, and hydrogen peroxide (H2O2) as the oxidant, are receiving increasing attention. This is due to their promising use as power sources for space and underwater applications, where air is not available and gas storage poses obvious problems. One key factor to improve the performance of DBFCs concerns the type of separator used. Both anion- and cation-exchange membranes may be considered as potential separators for DBFC. In the present paper, the effect of the membrane type on the performance of laboratory NaBH4/H2O2 fuel cells using Pt electrodes is studied at room temperature. Two commercial ion-exchange membranes from Membranes International Inc., an anion-exchange membrane (AMI-7001S) and a cation-exchange membrane (CMI-7000S), are tested as ionic separators for the DBFC. The membranes are compared directly by the observation and analysis of the corresponding DBFC's performance. Cell polarization, power density, stability, and durability tests are used in the membranes' evaluation. Energy densities and specific capacities are estimated. Most tests conducted, clearly indicate a superior performance of the cation-exchange membranes over the anion-exchange membrane. The two membranes are also compared with several other previously tested commercial membranes. For long term cell operation, these membranes seem to outperform the stability of the benchmark Nafion membranes but further studies are still required to improve their instantaneous power load. PMID:24958292

  5. Cu3-xP Nanocrystals as a Material Platform for Near-Infrared Plasmonics and Cation Exchange Reactions

    PubMed Central

    2015-01-01

    Synthesis approaches to colloidal Cu3P nanocrystals (NCs) have been recently developed, and their optical absorption features in the near-infrared (NIR) have been interpreted as arising from a localized surface plasmon resonance (LSPR). Our pump–probe measurements on platelet-shaped Cu3-xP NCs corroborate the plasmonic character of this absorption. In accordance with studies on crystal structure analysis of Cu3P dating back to the 1970s, our density functional calculations indicate that this material is substoichiometric in copper, since the energy of formation of Cu vacancies in certain crystallographic sites is negative, that is, they are thermodynamically favored. Also, thermoelectric measurements point to a p-type behavior of the majority carriers from films of Cu3-xP NCs. It is likely that both the LSPR and the p-type character of our Cu3-xP NCs arise from the presence of a large number of Cu vacancies in such NCs. Motivated by the presence of Cu vacancies that facilitate the ion diffusion, we have additionally exploited Cu3-xP NCs as a starting material on which to probe cation exchange reactions. We demonstrate here that Cu3-xP NCs can be easily cation-exchanged to hexagonal wurtzite InP NCs, with preservation of the anion framework (the anion framework in Cu3-xP is very close to that of wurtzite InP). Intermediate steps in this reaction are represented by Cu3-xP/InP heterostructures, as a consequence of the fact that the exchange between Cu+ and In3+ ions starts from the peripheral corners of each NC and gradually evolves toward the center. The feasibility of this transformation makes Cu3-xP NCs an interesting material platform from which to access other metal phosphides by cation exchange. PMID:25960605

  6. Transport of a reactive tracer in saturated alluvium described using a three-component cation-exchange model.

    PubMed

    Sullivan, Enid J; Reimus, Paul W; Counce, Dale A

    2003-01-01

    A weakly sorbing cation, lithium, will be used as a reactive tracer in upcoming field tracer tests in the saturated alluvium south of Yucca Mountain, Nevada. One objective of the field tests is to determine how well field-scale reactive transport can be predicted using transport parameters derived from laboratory experiments. This paper describes several laboratory lithium batch sorption and column transport experiments that were conducted using ground water and alluvium obtained from the site of the planned field tests. In the batch experiments, isotherms were determined over 2.5 orders of magnitude of lithium concentrations, corresponding to the range expected in the field tests. In addition to measuring equilibrium lithium concentrations, concentrations of other cations, namely Na(+), K(+), and Ca(2+), were measured in the batch tests to determine Li(+)-exchangeable equilibria. This information was used in conjunction with alluvium cation exchange capacity measurements to parameterize a three-component cation-exchange model (EQUIL) that describes lithium sorption in the alluvium system. This model was then applied to interpret the transport behavior of lithium ion in saturated alluvium column tests conducted at three different lithium bromide injection concentrations. The concentrations were selected such that lithium ion either dominated, accounted for a little over half, or accounted for only a small fraction of the total cation equivalents in the injection solution. Although tracer breakthrough curves differed significantly under each of these conditions, with highly asymmetric responses occurring at the highest injection concentrations, the three-component cation-exchange model reproduced the observed transport behavior of lithium and the other cations in each case with a similar set of model parameters. In contrast, a linear K(d)-type sorption model could only match the lithium responses at the lowest injection concentration. The three-component model will

  7. Anion- or Cation-Exchange Membranes for NaBH4/H2O2 Fuel Cells?

    PubMed Central

    Šljukić, Biljana; Morais, Ana L.; Santos, Diogo M. F.; Sequeira, César A. C.

    2012-01-01

    Direct borohydride fuel cells (DBFC), which operate on sodium borohydride (NaBH4) as the fuel, and hydrogen peroxide (H2O2) as the oxidant, are receiving increasing attention. This is due to their promising use as power sources for space and underwater applications, where air is not available and gas storage poses obvious problems. One key factor to improve the performance of DBFCs concerns the type of separator used. Both anion- and cation-exchange membranes may be considered as potential separators for DBFC. In the present paper, the effect of the membrane type on the performance of laboratory NaBH4/H2O2 fuel cells using Pt electrodes is studied at room temperature. Two commercial ion-exchange membranes from Membranes International Inc., an anion-exchange membrane (AMI-7001S) and a cation-exchange membrane (CMI-7000S), are tested as ionic separators for the DBFC. The membranes are compared directly by the observation and analysis of the corresponding DBFC’s performance. Cell polarization, power density, stability, and durability tests are used in the membranes’ evaluation. Energy densities and specific capacities are estimated. Most tests conducted, clearly indicate a superior performance of the cation-exchange membranes over the anion-exchange membrane. The two membranes are also compared with several other previously tested commercial membranes. For long term cell operation, these membranes seem to outperform the stability of the benchmark Nafion membranes but further studies are still required to improve their instantaneous power load. PMID:24958292

  8. Preparation of decarboxylic-functionalized weak cation exchanger and application for simultaneous separation of alkali, alkaline earth and transition metals.

    PubMed

    Peng, Yahui; Gan, Yihui; He, Chengxia; Yang, Bingcheng; Guo, Zhimou; Liang, Xinmiao

    2016-06-01

    A novel weak cation exchanger (WCX) with dicarboxyl groups functionalized has been developed by clicking mercaptosuccinic acid onto silica gel. The simple synthesis starts with modification of silica gel with triethoxyvinylsilane, followed by efficient coupling vinyl-bonded silica with mercaptosuccinic acid via a "thiol-ene" click reaction. The obtained WCX demonstrated good separation and high selectivity towards common metals. Simultaneous separation of 10 alkali, alkaline earth and transition metals was achieved within 12min. Ion exchange and complex mechanism dominates the separation process. Its utility was demonstrated for determination of metals in tap water. PMID:27130093

  9. Hydrazine-promoted sequential cation exchange: a novel synthesis method for doped ternary semiconductor nanocrystals with tunable emission.

    PubMed

    Shao, Haibao; Wang, Chunlei; Xu, Shuhong; Jiang, Yuan; Shao, Yujie; Bo, Fan; Wang, Zhuyuan; Cui, Yiping

    2014-01-17

    Using ZnSe nanocrystals (NCs) as starting material, Ag-doped or Cu-doped ZnCdSe ternary NCs were prepared by hydrazine-promoted sequential cation exchange in aqueous media. The composition of the NCs can be flexibly controlled by varying the amount of intermediate Ag or Cu cation addition, thus changing the emission of the ternary NCs while preserving the NC size. According to Vegard's law, the as-prepared ternary NCs possess an alloyed structure. In addition, the ternary NCs obtained have a high quantum yield, strong stability and a broad optical tuning range. PMID:24334495

  10. Atomic Resolution Monitoring of Cation Exchange in CdSe-PbSe Heteronanocrystals during Epitaxial Solid–Solid–Vapor Growth

    PubMed Central

    2014-01-01

    Here, we show a novel solid–solid–vapor (SSV) growth mechanism whereby epitaxial growth of heterogeneous semiconductor nanowires takes place by evaporation-induced cation exchange. During heating of PbSe-CdSe nanodumbbells inside a transmission electron microscope (TEM), we observed that PbSe nanocrystals grew epitaxially at the expense of CdSe nanodomains driven by evaporation of Cd. Analysis of atomic-resolution TEM observations and detailed atomistic simulations reveals that the growth process is mediated by vacancies. PMID:24844280

  11. Swelling and electro-osmotic properties of cation-exchange membranes with different structures in methanol-water media

    NASA Astrophysics Data System (ADS)

    Barragán, V. M.; Villaluenga, J. P. G.; Godino, M. P.; Izquierdo-Gil, M. A.; Ruiz-Bauzá, C.; Seoane, B.

    Electro-osmosis experiments through three cation-exchange membranes with different morphology and similar electric properties have been performed using methanol-water solutions under different experimental conditions. The influence on the electro-osmotic transport of the percentage of methanol on solvent with two different electrolytes, NaCl and LiCl, has been studied. The experimental results show that the presence of methanol in the solutions affects strongly the electro-osmotic flow, and this influence is different depending on the membrane morphology. Correlations among electro-osmotic permeability, swelling behavior, and cell resistance are studied for these membrane systems at different percentages of methanol in solvent.

  12. Cation exchange reactions controlling desorption of 90Sr 2+ from coarse-grained contaminated sediments at the Hanford site, Washington

    NASA Astrophysics Data System (ADS)

    McKinley, J. P.; Zachara, J. M.; Smith, S. C.; Liu, C.

    2007-01-01

    Nuclear waste that bore 90Sr 2+ was accidentally leaked into the vadose zone at the Hanford site, and was immobilized at relatively shallow depths in sediments containing little apparent clay or silt-sized components. Sr 2+, 90Sr 2+, Mg 2+, and Ca 2+ was desorbed and total inorganic carbon concentration was monitored during the equilibration of this sediment with varying concentrations of Na +, Ca 2+. A cation exchange model previously developed for similar sediments was applied to these results as a predictor of final solution compositions. The model included binary exchange reactions for the four operant cations and an equilibrium dissolution/precipitation reaction for calcite. The model successfully predicted the desorption data. The contaminated sediment was also examined using digital autoradiography, a sensitive tool for imaging the distribution of radioactivity. The exchanger phase containing 90Sr was found to consist of smectite formed from weathering of mesostasis glass in basaltic lithic fragments. These clasts are a significant component of Hanford formation sands. The relatively small but significant cation exchange capacity of these sediments was thus a consequence of reaction with physically sequestered clays in sediment that contained essentially no fine-grained material. The nature of this exchange component explained the relatively slow (scale of days) evolution of desorption solutions. The experimental and model results indicated that there is little risk of migration of 90Sr 2+ to the water table.

  13. Cation Exchange Reactions Controlling Desorption of 90Sr2+ From Coarse-Grained Contaminated Sediments at the Hanford Site, Washington

    NASA Astrophysics Data System (ADS)

    McKinley, J. P.; Zachara, J. M.; Smith, S. C.; Liu, C.

    2005-12-01

    Nuclear waste that bore 90Sr2+ was accidentally leaked into the vadose zone at the Hanford site, and was immobilized at relatively shallow depths in sediments containing little apparent clay or silt-sized components. We desorbed Sr2+, 90Sr2+, Mg2+, and Ca2+, and monitored total inorganic carbon concentration during the equilibration of this sediment with varying concentrations of Na+ and Ca2+. A cation exchange model previously developed for similar sediments was applied to these results as a predictor of final solution compositions. The model included binary exchange reactions for the four operant cations and an equilibrium dissolution/precipitation reaction for calcite. The model produced an excellent prediction for desorption data. We also examined the contaminated sediment using digital autoradiography, a sensitive tool for imaging the distribution of radioactivity. The exchanger phase containing 90Sr was found to consist of smectite formed from weathering of mesostasis glass in basaltic lithic fragments. These clasts are a significant component of Hanford formation sands. The relatively small but significant cation exchange capacity of these sediments was thus a consequence of reaction with physically sequestered clays in a sediment that contained essentially no fine-grained material. The nature of this exchange component explains the relatively slow (scale of days) evolution of desorption solutions. The experimental and model results indicate that there is little risk of migration of 90Sr2+ to the water table.

  14. Toward Separating Alpha-lactalbumin and Beta-lactoglobulin Proteins from Whey through Cation-exchange Adsorption

    NASA Astrophysics Data System (ADS)

    El-Sayed, Mayyada; Chase, Howard

    2009-05-01

    This paper describes the cation-exchange adsorption of the two major whey proteins, alpha-lactalbumin (ALA) and beta-lactoglobulin (BLG) with the purpose of establishing a process for isolating them from cow's milk whey. The single- and two-component adsorption of 1.5 mg/ml ALA and 3 mg/ml BLG to the cation-exchanger SP Sepharose FF at 20° C using 0.1 M acetate buffer of pH 3.7 was studied. Langmuir isotherm parameters were determined for the pure proteins. In two-component systems, BLG breakthrough curve exhibited an overshoot phenomenon that gave evidence for the presence of a competitive adsorption between the two proteins. Complete separation occurred and it was possible to obtain each of the two proteins in a pure form. The process was then applied to a whey concentrate mixture where incomplete separation took place. However, BLG was produced with 95% purity and a recovery of 80%, while ALA showed an 84% recovery with low purity.

  15. In-situ graft-polymerization preparation of cation-exchange supermacroporous cryogel with sulfo groups in glass columns.

    PubMed

    Yao, Kejian; Yun, Junxian; Shen, Shaochuan; Chen, Fang

    2007-07-20

    Graft polymerization of monomer chains with expected functional groups onto the matrix pore surfaces by initiator is an effective approach for introducing ion-exchange groups to cryogel matrix to get anion- or cation-exchange supermacroporous cryogels. In this work, a novel cation-exchange cryogel with sulfo binding groups was prepared by grafting of 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPSA) onto polyacrylamide-based cryogels in glass columns. The grafting polymerization was achieved in an in-situ manner which was performed by pumping the initiator and the reactive solution of graft monomer with sulfo binding groups directly through a cryogel bed pre-produced in a glass column under frozen condition. The axial liquid dispersion characteristics within the monolithic cryogel beds before and after the in-situ polymerization were compared by measuring residence time distributions (RTDs) at various liquid flow rates using tracer pulse-response method. Microstructure morphology of pores within cryogels was analyzed by scanning electron microscopy (SEM). Chromatography of lysozyme was carried out to reveal the protein breakthrough and elution characteristics in the obtained cryogel beds. PMID:17517417

  16. Uncertainties of Gaseous Oxidized Mercury Measurements Using KCl-Coated Denuders, Cation-Exchange Membranes, and Nylon Membranes: Humidity Influences.

    PubMed

    Huang, Jiaoyan; Gustin, Mae Sexauer

    2015-05-19

    Quantifying the concentration of gaseous oxidized mercury (GOM) and identifying the chemical compounds in the atmosphere are important for developing accurate local, regional, and global biogeochemical cycles. The major hypothesis driving this work was that relative humidity affects collection of GOM on KCl-coated denuders and nylon membranes, both currently being applied to measure GOM. Using a laboratory manifold system and ambient air, GOM capture efficiency on 3 different collection surfaces, including KCl-coated denuders, nylon membranes, and cation-exchange membranes, was investigated at relative humidity ranging from 25 to 75%. Recovery of permeated HgBr2 on KCl-coated denuders declined by 4-60% during spikes of relative humidity (25 to 75%). When spikes were turned off GOM recoveries returned to 60 ± 19% of permeated levels. In some cases, KCl-coated denuders were gradually passivated over time after additional humidity was applied. In this study, GOM recovery on nylon membranes decreased with high humidity and ozone concentrations. However, additional humidity enhanced GOM recovery on cation-exchange membranes. In addition, reduction and oxidation of elemental mercury during experiments was observed. The findings in this study can help to explain field observations in previous studies. PMID:25877790

  17. DC conductivity, cationic exchange capacity, and specific surface area related to chemical composition of pore lining chlorites.

    PubMed

    Henn, François; Durand, Claudine; Cerepi, Adrian; Brosse, Etienne; Giuntini, J C

    2007-07-15

    Low resistivity in argillaceous sandstone reservoirs may be attributed either to the effect of microporosity, or to specific effects due to intrinsic clays' conducting properties or to other conducting minerals. In order to distinguish these effects, cation exchange capacity, specific surface areas, and dc conductivity of various pore lining chlorite-bearing sandstones from different hydrocarbon reservoir measurements are investigated. Cation exchange capacity and specific surface area are measured on whole rocks as well as on size-separated fractions. Both sets of values are low, in agreement with the structural and textural observations. The conductivity of these chlorites, measured in air conditions and after dehydration, is investigated by means of complex impedance spectroscopy on size-separated fractions as a function of temperature and compared to that of reference clays. The results show a large influence of moisture, applied electric field frequency, and temperature on the electrical properties. The magnitude of the dehydrated clays' conductivity is such that its influence on the conductivity of argillaceous sandstone is lower than that related to the presence of water or brine by several orders of magnitude. The dc conductivity and the related activation energy of the dehydrated samples appear to be related to the chemical composition of the clays. More specifically, a clear correlation occurs with the electrical charges of the clay network, that is to say with the location, i.e., tetrahedral or octahedral sites, of the substituting trivalent elements. PMID:17433348

  18. [Enhanced Performance of Rolled Membrane Electrode Assembly by Adding Cation Exchange Resin to Anode in Microbial Fuel Cells].

    PubMed

    Mei, Zhuo; Zhang, Zhe; Wang, Xin

    2015-11-01

    The membrane electrode assembly (MEA) with an anode-membrane-cathode structure ban reduce the distance between anode and cathode to improve the power of microbial fuel cells (MFCs). Here in order to further promote the performance of MFCs, a novel MEA was constructed by rolling-press method without noble metal material, and the Ohmic resistance decreased to 3-5 Ω. The maximum power density was 446 mW x m(-2) when acetate was used as the substrate. Solid spheres (like polystyrene balls and glass microspheres) were added into anode to enhance the transportation of electrolyte to cathode, resulting in a 10% increase in power density by producing macropores on and in the anode during rolling process. Cation exchange resin was added to accelerate the transportation of proton through the anode so that the power density further increased to 543 mW x m(-2). Meanwhile, the stability of cell voltage and Coulomb efficiency of MFC were both enhanced after the addition of cation exchange resin. PMID:26911023

  19. Damping Behavior of Alumina Epoxy Nano-Composites

    NASA Astrophysics Data System (ADS)

    Katiyar, Priyanka; Kumar, Anand

    2016-05-01

    Polymer nano composites, consisting of a polymer matrix with nanoparticle filler, have been predicted to be one of the most beneficial applications of nanotechnology. Addition of nano particulates to a polymer matrix enhances its performance by capitalizing on the nature and properties of the nano-scale fillers. The damping behavior of composites with nano structured phases is significantly different from that of micro structured materials. Viscoelastic homopolymer exhibit a high material damping response over a relatively narrow range of temperature and frequencies. In many practical situations, a polymeric structure is required to possess better strength and stiffness properties together with a reasonable damping behavior. Viscoelastic polymers show higher loss factor beyond the glassy region which comes with a significant drop in the specific modulus. Addition of nano alumina particles to epoxy leads to improved strength and stiffness properties with an increase in glass transition temperature while retaining its damping capability. Experimental investigations are carried out on composite beam specimen fabricated with different compositions of alumina nano particles in epoxy to evaluate loss factor, tan δ. Impact damping method is used for time response analysis. A single point Laser is used to record the transverse displacement of a point on the composite beam specimen. The experimental results are compared with theoretical estimation of loss factor using Voigt estimation. The effect of inter phase is included in theoretical estimation of loss factor. The result reveals that the study of interface properties is very important in deriving the overall loss factor of the composite since interface occupies a significant volume fraction in the composite.

  20. Chromatographic evaluation of reversed-phase/anion-exchange/cation-exchange trimodal stationary phases prepared by electrostatically driven self-assembly process.

    PubMed

    Liu, Xiaodong; Pohl, Christopher; Woodruff, Andrew; Chen, Jinhua

    2011-06-01

    This work describes chromatographic properties of reversed-phase/cation-exchange/anion-exchange trimodal stationary phases. These stationary phases were based on high-purity porous spherical silica particles coated with nano-polymer beads using an electrostatically driven self-assembly process. The inner-pore area of the material was modified covalently with an organic layer that provided both reversed-phase and anion-exchange properties while the outer surface was coated with nano-sized polymer beads with strong cation-exchange characteristics. This design ensured spatial separation of the anion-exchange and the cation-exchange regions, and allowed reversed-phase, anion-exchange and cation-exchange retention mechanisms to function simultaneously. Chromatographic evaluation of ions and small molecules suggested that retention of ionic analytes was influenced by the ionic strength, pH, and mobile phase organic solvent content, and governed by both ion-exchange and hydrophobic interactions. Meanwhile, neutral analytes were retained by hydrophobic interaction and was mainly affected by mobile phase organic solvent content. Depending on the specific application, selectivity could be optimized by adjusting the anion-exchange/cation-exchange capacity ratio (selectivity), which was achieved experimentally by using porous silica particles with different surface areas. PMID:21530974

  1. Preparation and photocatalytic properties of AgI–SnO{sub 2} nano-composites

    SciTech Connect

    Wen, Biao; Wang, Xiao-Hui; Lu, Juan; Cao, Jia-Lei; Wang, Zuo-Shan

    2013-05-15

    Highlights: ► AgI–SnO{sub 2} nano-composites have been successfully synthesized. ► As-prepared AgI–SnO{sub 2} nano-composites own the excellent visible light photocatalytic activity. ► As-prepared AgI–SnO{sub 2} nano-composites own the excellent stability. - Abstract: AgI doped SnO{sub 2} nano-composites were prepared by the chemical coprecipitation method and were characterized by the X-ray diffraction, transmission electron microscopy and X-ray photoelectron spectroscopy. Results showed that main of the I{sup −} ions remained in the AgI lattice which is highly dispersed in the system. The photo-catalytic experiments performed under visible light irradiation using methylene blue as the pollutant revealed that not only the photo-catalytic activity but also the stability of SnO{sub 2} based photocatalyst could be improved by introduction of an appropriate amount of AgI, and the result was further supported by the UV–Vis diffuse reflection spectra and the electron spin-resonance spectra. Among all of the samples, AgI–SnO{sub 2} nano-composite with 2At% AgI exhibited the best catalytic efficiency and stability.

  2. Biochar-based nano-composites for the decontamination of wastewater: A review.

    PubMed

    Tan, Xiao-Fei; Liu, Yun-Guo; Gu, Yan-Ling; Xu, Yan; Zeng, Guang-Ming; Hu, Xin-Jiang; Liu, Shao-Bo; Wang, Xin; Liu, Si-Mian; Li, Jiang

    2016-07-01

    Synthesizing biochar-based nano-composites can obtain new composites and combine the advantages of biochar with nano-materials. The resulting composites usually exhibit great improvement in functional groups, pore properties, surface active sites, catalytic degradation ability and easy to separation. These composites have excellent abilities to adsorb a range of contaminants from aqueous solutions. Particularly, catalytic material-coated biochar can exert simultaneous adsorption and catalytic degradation function for organic contaminants removal. Synthesizing biochar-based nano-composites has become an important practice for expanding the environmental applications of biochar and nanotechnology. This paper aims to review and summarize the various synthesis techniques for biochar-based nano-composites and their effects on the decontamination of wastewater. The characteristic and advantages of existing synthesis methods are summarized and discussed. Application of biochar-based nano-composites for different contaminants removal and the underlying mechanisms are reviewed. Furthermore, knowledge gaps that exist in the fabrication and application of biochar-based nano-composites are also identified. PMID:27131871

  3. Chemically synthesized nano composite (Zinc/Magnesium) Oxide for tunable band gap devices

    NASA Astrophysics Data System (ADS)

    Sharmila, P. P.; Tharayil, Nisha J.

    2015-02-01

    Formation of hetro structures in nano structured materials is essential for their potential applications in nano electronics and photonic devices. As a promising candidate for blue and ultraviolet optoelectronic devices, ZnO has attracted much attention due to its wide band gap (3.37eV), large exciton binding energy (60meV), low epitaxial growth temperature and high oxidation resistance. In addition since the ionic radii of Mg+2+(0.57A0) and Zn2+(0.60A0) are quite close, they may alloy by replacing each other in the matrix. The doping of Mg in ZnO is done through a simple and novel technique from metal acetates using ammonium carbonate as precipitant. An organic capping agent (EDTA) is used prevent agglomeration and the addition is done under constant stirring. The carbonate precursor obtained is heated on the basis of TGA to obtain the metal nano composite. The effects of different parameters on particle size and morphology of (Zn-Mg)O nano composite is optimized by "one at a time" method. Under optimum conditions, spongy shaped, uniform and homogeneous structured (Zn-Mg)O nano composite powders with particle size few nano meters are obtained. The optical and structural properties of nano composite prepared by solution techniques are investigated by X-ray diffraction, UV-Visible spectroscopy, and PL, FTIR and electron microscopy techniques. The effect of annealing on the optical properties of this nano composite is also studied

  4. Formation of ZnSe/Bi{sub 2}Se{sub 3} QDs by surface cation exchange and high photothermal conversion

    SciTech Connect

    Jia, Guozhi; Wang, Peng; Zhang, Yanbang; Wu, Zengna; Li, Qiang; Yao, Jianghong; Chang, Kai

    2015-08-15

    Water-dispersed core/shell structure ZnSe/Bi{sub 2}Se{sub 3} quantum dots were synthesized by ultrasonicwave-assisted cation exchange reaction. Only surface Zn ion can be replaced by Bi ion in ZnSe quantum dots, which lead to the ultrathin Bi{sub 2}Se{sub 3} shell layer formed. It is significance to find to change the crystal of QDs due to the acting of ultrasonicwave. Cation exchange mechanism and excellent photothermal conversion properties are discussed in detail.

  5. Preparation and evaluation of rigid porous polyacrylamide-based strong cation-exchange monolithic columns for capillary electrochromatography.

    PubMed

    Dong, Jing; Ou, Junjie; Dong, Xiaoli; Wu, Renan; Ye, Mingliang; Zou, Hanfa

    2007-11-01

    A CEC monolithic column with strong cation-exchange (SCX) stationary phase based on hydrophilic monomers was prepared by in situ polymerization of acrylamide, methylenebisacrylamide, and 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS) in a complete organic binary porogenic solvent consisting of DMSO and dodecanol. The sulfonic groups provided by the monomer AMPS on the surface of the stationary phase generate an EOF from anode to cathode, and serve as an SCX stationary phase at the same time. The monolithic stationary phase exhibited normal-phase chromatographic behavior for neutral analytes. For charged analytes, electrostatic interaction/repulsion with the monolith was observed. The strong SCX monolithic column has been successfully employed in the electrochromatographic separation of basic drugs, peptides, and alkaloids extracted from natural products. PMID:17924588

  6. Full cell study of Diels Alder poly(phenylene) anion and cation exchange membranes in vanadium redox flow batteries

    DOE PAGESBeta

    Pezeshki, Alan M.; Fujimoto, Cy; Sun, Che -Nan; Mench, Matthew M.; Zawodzinski, Thomas A.; Tang, Z. J.

    2015-11-14

    In this paper, we report on the performance of Diels Alder poly(phenylene) membranes in vanadium redox flow batteries. The membranes were functionalized with quaternary ammonium groups to form an anion exchange membrane (QDAPP) and with sulfonic acid groups to form a cation exchange membrane (SDAPP). Both membrane classes showed similar conductivities in the battery environment, suggesting that the ion conduction mechanism in the material is not strongly affected by the moieties along the polymer backbone. The resistance to vanadium permeation in QDAPP was not improved relative to SDAPP, further suggesting that the polarity of the functional groups do not playmore » a significant role in the membrane materials tested. Both QDAPP and SDAPP outperformed Nafion membranes in cycling tests, with both achieving voltage efficiencies above 85% while maintaining 95% coulombic efficiency while at a current density of 200 mA/cm2.« less

  7. Full cell study of Diels Alder poly(phenylene) anion and cation exchange membranes in vanadium redox flow batteries

    SciTech Connect

    Pezeshki, Alan M.; Fujimoto, Cy; Sun, Che -Nan; Mench, Matthew M.; Zawodzinski, Thomas A.; Tang, Z. J.

    2015-11-14

    In this paper, we report on the performance of Diels Alder poly(phenylene) membranes in vanadium redox flow batteries. The membranes were functionalized with quaternary ammonium groups to form an anion exchange membrane (QDAPP) and with sulfonic acid groups to form a cation exchange membrane (SDAPP). Both membrane classes showed similar conductivities in the battery environment, suggesting that the ion conduction mechanism in the material is not strongly affected by the moieties along the polymer backbone. The resistance to vanadium permeation in QDAPP was not improved relative to SDAPP, further suggesting that the polarity of the functional groups do not play a significant role in the membrane materials tested. Both QDAPP and SDAPP outperformed Nafion membranes in cycling tests, with both achieving voltage efficiencies above 85% while maintaining 95% coulombic efficiency while at a current density of 200 mA/cm2.

  8. The investigation on cationic exchange capacity of zeolites: the use as selective ion trappers in the electrokinetic soil technique.

    PubMed

    Ursini, Ornella; Lilla, Edo; Montanari, Roberta

    2006-09-21

    The cation exchange capacity (CEC) of porous zeolites allows to adsorb in the framework cavities the cations as pollutant heavy metal ions. We investigate the CEC behaviour of different zeolites in different experimental conditions; in solution where the ion's mobility is spontaneous and free and in the electrokinetic system where the ion's mobility is driven by the electric field. The aim of this study is to investigate if the CEC is an useful property to create a special interface region of zeolites, that if placed in the electrokinetic cell, just before the cathode, could allow to capture and concentrate the heavy metallic ions, during their migrating process. The zeolite 13X investigated in the electrokinetic proofs, retains a good high ions adsorption, even if quite smaller than the relevant free solution condition and well acts as confined trap for the heavy metal ions. In fact no trace of metallic deposition are present on the electrode's surface. PMID:16716501

  9. Tree species affect cation exchange capacity (CEC) and cation binding properties of organic matter in acid forest soils.

    PubMed

    Gruba, Piotr; Mulder, Jan

    2015-04-01

    Soil organic matter (SOM) in forest soil is of major importance for cation binding and acid buffering, but its characteristics may differ among soils under different tree species. We investigated acidity, cation exchange properties and Al bonding to SOM in stands of Scots pine, pedunculate oak, Norway spruce, European beech and common hornbeam in southern Poland. The content of total carbon (Ct) was by far the major contributor to total cation exchange capacity (CECt) even in loamy soils and a strong relationship between Ct and CECt was found. The slope of the regression of CECt to Ct increased in the order hornbeam≈oak

  10. Fibrous polymer grafted magnetic chitosan beads with strong poly(cation-exchange) groups for single step purification of lysozyme.

    PubMed

    Bayramoglu, Gulay; Tekinay, Turgay; Ozalp, V Cengiz; Arica, M Yakup

    2015-05-15

    Lysozyme is an important polypetide used in medical and food applications. We report a novel magnetic strong cation exchange beads for efficient purification of lysozyme from chicken egg white. Magnetic chitosan (MCHT) beads were synthesized via phase inversion method, and then grafted with poly(glycidyl methacrylate) (p(GMA)) via the surface-initiated atom transfer radical polymerization (SI-ATRP). Epoxy groups of the grafted polymer, were modified into strong cation-exchange groups (i.e., sulfonate groups) in the presence of sodium sulfite. The MCTH and MCTH-g-p(GMA)-SO3H beads were characterized by ATR-FTIR, SEM, and VSM. The sulphonate groups content of the modified MCTH-g-p(GMA)-4 beads was found to be 0.53mmolg(-1) of beads by the potentiometric titration method. The MCTH-g-p(GMA)-SO3H beads were first used as an ion-exchange support for adsorption of lysozyme from aqueous solution. The influence of different experimental parameters such as pH, contact time, and temperature on the adsorption process was evaluated. The maximum adsorption capacity was found to be 208.7mgg(-1) beads. Adsorption of lysozyme on the MCTH-g-p(GMA)-SO3H beads fitted to Langmuir isotherm model and followed the pseudo second-order kinetic. More than 93% of the adsorbed lysozyme was desorbed using Na2CO3 solution (pH 11.0). The purity of the lysozyme was checked by HPLC and SDS gel electrophoresis. In addition, the MCTH-g-p(GMA)-SO3H beads prepared in this work showed promising potential for separation of various anionic molecules. PMID:25864009

  11. The group separation of the rare-earth elements and yttrium from geologic materials by cation-exchange chromatography

    USGS Publications Warehouse

    Crock, J.G.; Lichte, F.E.; Wildeman, T.R.

    1984-01-01

    Demand is increasing for the determination of the rare-earth elements (REE) and yttrium in geologic materials. Due to their low natural abundance in many materials and the interferences that occur in many methods of determination, a separation procedure utilizing gradient strong-acid cation-exchange chromatography is often used to preconcentrate and isolate these elements from the host-rock matrix. Two separate gradient strong-acid cation-exchange procedures were characterized and the major elements as well as those elements thought to provide the greatest interference for the determination of the REE in geologic materials were tested for separation from the REE. Simultaneous inductively coupled argon plasma-atomic emission spectroscopy (ICAP-AES) measurements were used to construct the chromatograms for the elution studies, allowing the elution patterns of all the elements of interest to be determined in a single fraction of eluent. As a rock matrix, U.S. Geological Survey standard reference BCR-1 basalt was digested using both an acid decomposition procedure and a lithium metaborate fusion. Hydrochloric and nitric acids were tested as eluents and chromatograms were plotted using the ICAP-AES data; and we observed substantial differences in the elution patterns of the REE and as well as in the solution patterns of Ba, Ca, Fe and Sr. The nitric acid elution required substantially less eluent to elute the REE and Y as a group when compared to the hydrochloric acid elution, and provided a clearer separation of the REE from interfering and matrix elements. ?? 1984.

  12. Room Temperature Cation Exchange Reaction in Nanocrystals for Ultrasensitive Speciation Analysis of Silver Ions and Silver Nanoparticles.

    PubMed

    Huang, Ke; Xu, Kailai; Tang, Jie; Yang, Lu; Zhou, Jingrong; Hou, Xiandeng; Zheng, Chengbin

    2015-07-01

    To evaluate the toxicity of silver nanoparticles (AgNPs) and Ag(+) and gain deep insight into the transformation of AgNPs in the environment or organisms, ultrasensitive analytical methods are needed for their speciation analysis. About 40-fold of Cd(2+) in CdTe ionic nanocrystals can be "bombarded-and-exploded" (exchanged) in less than 1 min simply by mixing the nanocrystals with Ag(+) solution at room temperature, while this cation exchange reaction did not occur when only silver nanoparticles were present. On the basis of this striking difference, an ultrasensitive method was developed for speciation analysis of Ag(+) and AgNPs in complex matrices. The released Cd(2+) was reduced to its volatile species by sodium tetrahydroborate, which was separated and swept to an inductively coupled plasma mass spectrometer (ICPMS) or an atomic fluorescence spectrometer (AFS) for the indirect but ultrasensitive detection of Ag(+). Owing to the remarkable signal amplification via the cation exchange reaction and the advantages of chemical vapor generation for sampling, the limit of detection was 0.0003 μg L(-1) for Ag(+) by ICPMS, which was improved by 100-fold compared to the conventional method. Relative standard deviations are better than 2.5% at a concentration of 0.5 μg L(-1) Ag(+) or AgNPs regardless of the detector. The proposed method retains several unique advantages, including ultrahigh sensitivity, speciation analysis, simplicity and being organic reagent-free, and has been successfully utilized for speciation analysis of Ag(+) and AgNPs in environmental water samples and paramecium cells. PMID:26017198

  13. Common Ion Effects In Zeoponic Substrates: Dissolution And Cation Exchange Variations Due to Additions of Calcite, Dolomite and Wollastonite

    NASA Technical Reports Server (NTRS)

    Beiersdorfer, R. E.; Ming, D. W.; Galindo, C., Jr.

    2003-01-01

    c1inoptilolite-rich tuff-hydroxyapatite mixture (zeoponic substrate) has the potential to serve as a synthetic soil-additive for plant growth. Essential plant macro-nutrients such as calcium, phosphorous, magnesium, ammonium and potassium are released into solution via dissolution of the hydroxyapatite and cation exchange on zeolite charged sites. Plant growth experiments resulting in low yield for wheat have been attributed to a Ca deficiency caused by a high degree of cation exchange by the zeolite. Batch-equilibration experiments were performed in order to determine if the Ca deficiency can be remedied by the addition of a second Ca-bearing, soluble, mineral such as calcite, dolomite or wollastonite. Variations in the amount of calcite, dolomite or wollastonite resulted in systematic changes in the concentrations of Ca and P. The addition of calcite, dolomite or wollastonite to the zeoponic substrate resulted in an exponential decrease in the phosphorous concentration in solution. The exponential rate of decay was greatest for calcite (5.60 wt. % -I), intermediate for wollastonite (2.85 wt.% -I) and least for dolomite (1.58 wt.% -I). Additions of the three minerals resulted in linear increases in the calcium concentration in solution. The rate of increase was greatest for calcite (3.64), intermediate for wollastonite (2.41) and least for dolomite (0.61). The observed changes in P and Ca concentration are consistent with the solubilities of calcite, dolomite and wollastonite and with changes expected from a common ion effect with Ca. Keywords: zeolite, zeoponics, common-ion effect, clinoptilolite, hydroxyapatite

  14. Adsorption of reovirus to clay minerals: effects of cation-exchange capacity, cation saturation, and surface area.

    PubMed Central

    Lipson, S M; Stotzky, G

    1983-01-01

    The adsorption of reovirus to clay minerals has been reported by several investigators, but the mechanisms defining this association have been studied only minimally. The purpose of this investigation was to elucidate the mechanisms involved with this interaction. More reovirus type 3 was adsorbed, in both distilled and synthetic estuarine water, by low concentrations of montmorillonite than by comparable concentrations of kaolinite containing a mixed complement of cations on the exchange complex. Adsorption to the clays was essentially immediate and was correlated with the cation-exchange capacity of the clays, indicating that adsorption was primarily to negatively charged sites on the clays. Adsorption was greater with low concentrations of clays in estuarine water than in distilled water, as the higher ionic strength of the estuarine water reduced the electrokinetic potential of both clay and virus particles. The addition of cations (as chloride salts) to distilled water enhanced adsorption, with divalent cations being more effective than monovalent cations and 10(-2) M resulting in more adsorption than 10(-3) M. Potassium ions suppressed reovirus adsorption to montmorillonite, probably by collapsing the clay lattices and preventing the expression of the interlayer-derived cation-exchange capacity. More virus was adsorbed by montmorillonite made homoionic to various mono-, di-, and trivalent cations (except by montmorillonite homoionic to potassium) than by comparable concentrations of kaolinite homoionic to the same cations. The sequence of the amount of adsorption to homoionic montmorillonite was Al greater than Ca greater than Mg greater than Na greater than K; the sequence of adsorption to kaolinite was Na greater than Al greater than Ca greater than Mg greater than K. The constant partition-type adsorption isotherms obtained when the clay concentration was maintained constant and the virus concentration was varied indicated that a fixed proportion of the

  15. Comparison of Reactive Mercury Concentrations Measured Simultaneously Using KCl-coated Denuders, Nylon Membranes, and Cation Exchange Membranes

    NASA Astrophysics Data System (ADS)

    Gustin, M. S.; Huang, J.; Miller, M. B.; Weiss-Penzias, P. S.

    2012-12-01

    There is much debate about the chemistry of reactive gaseous and particle bound mercury (Hg) in the atmosphere, and the processes associated with formation. In addition, there are concerns regarding the interferences and calibration of the widely used Tekran® 2537/1130/1135 Hg measurement system. To investigate these we developed simple laboratory and field sampling systems designed to collect and analyze reactive Hg (Hg (II), Hg (I) and/or particle bound). A manifold system was applied in the laboratory, and in the field, in-series and -parallel membranes, flow controllers and pumps were utilized. Both systems actively collected reactive Hg using nylon membranes and cation exchange membranes alongside measurements made using the Tekran® system. The analytical system consisted of step wise 2.5 minute thermo-desorption and Hg quantification by cold vapor atomic fluorescence. In the laboratory, we compared the efficiency of these surfaces for collection of HgO, HgCl2, and HgBr2 when permeated into Hg and oxidant free air, and ambient filtered air. Other tests are ongoing. Thus far, results show concentrations measured by the cation exchange membrane were two-to-three fold greater than that measured by the nylon membranes, and three-to -four fold greater than that measured by the KCl-coated annual denuder. Thermo-desorption profiles obtained using nylon membranes show slightly different patterns associated with the reactive Hg compounds as permeated and tested. Field measurements were made at two locations in Reno, Nevada (a high traffic site and an agricultural area) and at Elkhorn Slough, California (marine site). Desorption profiles from nylon membrane differed by site and by time of year. Although the influence of aerosol on this measurement has not been explored, field results suggest different forms of reactive Hg were present in the atmosphere as a function of season and location.

  16. Evolution of hollow TiO2 nanostructures via the Kirkendall effect driven by cation exchange with enhanced photoelectrochemical performance.

    PubMed

    Yu, Yanhao; Yin, Xin; Kvit, Alexander; Wang, Xudong

    2014-05-14

    Hollow nanostructures are promising building blocks for electrode scaffolds and catalyst carriers in energy-related systems. In this paper, we report a discovery of hollow TiO2 nanostructure evolution in a vapor-solid deposition system. By introducing TiCl4 vapor pulses to ZnO nanowire templates, we obtained TiO2 tubular nanostructures with well-preserved dimensions and morphology. This process involved the cation exchange reaction between TiCl4 vapor and ZnO solid and the diffusion of reactants and products in their vapor or solid phases, which was likely a manifestation of the Kirkendall effect. The characteristic morphologies and the evolution phenomena of the hollow nanostructures from this vapor-solid system were in a good agreement with the Kirkendall effect discovered in solution systems. Complex hollow TiO2 nanostructures were successfully acquired by replicating various ZnO nanomorphologies, suggesting that this unique cation exchange process could also be a versatile tool for nanostructure replication in vapor-solid growth systems. The evolution of TiO2 nanotubes from ZnO NW scaffolds was seamlessly integrated with TiO2 NR branch growth and thus realized a pure TiO2-phased 3D NW architecture. Because of the significantly enlarged surface area and the trace amount of Zn left in the TiO2 crystals, such 3D TiO2 nanoforests demonstrated enhanced photoelectrochemical performance particularly under AM (air mass) 1.5G illumination, offering a new route for hierarchical functional nanomaterial assembly and application. PMID:24679077

  17. Advance chromatin extraction enhances performance and productivity of cation exchange chromatography-based capture of Immunoglobulin G monoclonal antibodies.

    PubMed

    Nian, Rui; Gagnon, Pete

    2016-07-01

    The impact of host cell-derived chromatin was investigated on the performance and productivity of cation exchange chromatography as a method for capture-purification of an IgG monoclonal antibody. Cell culture supernatant was prepared for loading by titration to pH 6.0, dilution with water to a conductivity of 4mS/cm, then microfiltration to remove solids. DNA content was reduced 99% to 30ppm, histone host cell protein content by 76% to 6300ppm, non-histone host cell protein content by 15% to 321,000ppm, and aggregates from 33% to 15%. IgG recovery was 83%. An alternative preparation was performed, adding octanoic acid, allantoin, and electropositive particles to the harvest at pH 5.3, then removing solids. DNA content was reduced to<1 ppb, histones became undetectable, non-histones were reduced to 24,000ppm, and aggregates were reduced to 2.4%. IgG recovery was 95%. This treatment increased dynamic capacity (DBC) of cation exchange capture to 173g/L and enabled the column to reduce non-histone host proteins to 671ppm. Step recovery was 99%. A single multimodal polishing step further reduced them to 15ppm and aggregates to <0.1%. Overall process recovery was 89%. Productivity at feed stream IgG concentrations of 5-10g/L was roughly double the productivity of a same-size protein A column with a DBC of 55g/L. PMID:27247214

  18. Analytical cation-exchange chromatography to assess the identity, purity, and N-terminal integrity of human lactoferrin.

    PubMed

    van Veen, Harrie A; Geerts, Marlieke E J; van Berkel, Patrick H C; Nuijens, Jan H

    2002-10-01

    Human lactoferrin (hLF) is an iron-binding glycoprotein involved in the innate host defense. The positively charged N-terminal domain of hLF mediates several of its activities by interacting with ligands such as bacterial lipopolysaccharide (LPS), specific receptors, and other proteins. This cationic domain is highly susceptible to limited proteolysis, which impacts on the affinity of hLF for the ligand. An analytical method, employing cation-exchange chromatography on Mono S, was developed to assess the N-terminal integrity of hLF preparations. The method, which separates N-terminally intact hLF from hLF species lacking two (Gly(1)-Arg(2)) or three (Gly(1)-Arg(2)-Arg(3)) residues, showed that 5-58% of total hLF in commercially obtained preparations was N-terminally degraded. The elution profile of hLF on Mono S unequivocally differed from lactoferrins from other species as well as homologous and other whey proteins. Analysis of fresh human whey samples revealed two variants of N-terminally intact hLF, but not limitedly proteolyzed hLF. Mono S chromatography of 2 out of 26 individual human whey samples showed a rare polymorphic hLF variant with three N-terminal arginines (Gly(1)-Arg(2)-Arg(3)-Arg(4)-Ser(5)-) instead of the usual variant with four N-terminal arginines (Gly(1)-Arg(2)-Arg(3)-Arg(4)-Arg(5)-Ser(6)-). In conclusion, Mono S cation-exchange chromatography appeared a robust method to assess the identity, purity, N-terminal integrity, and the presence of polymorphic and intact hLF variants. PMID:12381362

  19. Quantification of melamine in human urine using cation-exchange based high performance liquid chromatography tandem mass spectrometry.

    PubMed

    Panuwet, Parinya; Nguyen, Johnny V; Wade, Erin L; D'Souza, Priya E; Ryan, P Barry; Barr, Dana Boyd

    2012-03-01

    Melamine and cyanuric acid have been implicated as adulterants in baby formula in China and pet foods in North America. In China, the effect of melamine or melamine-cyanuric acid adulteration lead to kidney stone development and acute renal failure in thousands of Chinese infants. A selective and sensitive analytical method was developed to measure melamine in human urine in order to evaluate the extent of potential health implications resulting from the consumption of these types of adulterated products in the general US population. This method involves extracting melamine from human urine using cation-exchange solid-phase extraction, chromatographically separating it from its urinary matrix co-extractants on a silica-based, strong-cation exchange analytical column using high performance liquid chromatography, and analysis using positive mode electrospray ionization tandem mass spectrometry. Quantification was performed using modified, matrix-based isotope dilution calibration covering the concentration range of 0.50-100 ng/mL. The limit of detection, calculated using replicates of blank and low level spiked samples, was 0.66 ng/mL and the relative standard deviations were between 6.89 and 14.9%. The relative recovery of melamine was 101-106%. This method was tested for viability by analyzing samples collected from the general US population. Melamine was detected in 76% of the samples tested, with a geometric mean of 2.37 ng/mL, indicating that this method is suitable for reliably detecting background exposures to melamine or other chemicals from which it can be derived. PMID:22309774

  20. Nonlocal theory and finite element modeling of nano-composites

    NASA Astrophysics Data System (ADS)

    Alvinasab, Ali

    This research is concerned with fundamentals of modeling nano-composites. The study contains two major parts, namely, numerical modeling of nanocomposites and nonlocal theory based approach for predicting behavior of Carbon Nanotubes (CNTs). Computational modeling of glass (silica) fibers having micro-scale outer dimensions and nano-scale internal structures was performed to assess its mechanical behavior. Self-assembly technique was used to synthesize the individual fibers of approximately 5 mum in length with a hexagonal cross-section (2mum between two opposite sides) and honeycomb-like internal nano-structures. These fibers have several potential applications including synthesis of multifunctional composite materials. Numerical modeling of the individual fibers was performed using continuum mechanics based approach wherein linear elastic elements were utilized within a commercial finite element (FE) analysis software. A representative volume element approach was adopted for computational efficiency. Appropriate loads and boundary conditions were used to derive stress-strain relationship (stiffness matrix) which has six independent constants for the individual fiber. Force-displacement relationships under simulated nanoindentation were obtained for the actual fiber (with six independent constants) and under transversely isotropic approximation. The contact problem was solved for the transversely isotropic case, which indicated a much stiffer fiber compared to the FE predictions. This difference is likely due to the geometric nonlinearity considered in FE analysis yielding accurate results for large displacements. The effective mechanical properties of randomly oriented nano-structured glass fiber composite are evaluated by using a continuum mechanics based FE model. The longitudinal and transverse properties of aligned fiber are calculated. Then the equivalent material properties for tilted fiber with different fiber orientations are obtained. Based on equivalent

  1. Acoustic properties of alumina colloidal/polymer nano-composite film on silicon.

    PubMed

    Zhang, Rui; Cao, Wenwu; Zhou, Qifa; Cha, Jung Hyui; Shung, K Kirk; Huang, Yuhong

    2007-03-01

    Alumina colloidal/polymer composite films on silicon substrates have been successfully fabricated using the sol-gel method, in which the crystallite sizes of alumina are between 20 and 50 nm. The density and ultrasonic phase velocities in these films with different alumina ratios from 14% to 32% were measured at the desired operating frequency. We have proved that the density, acoustic phase velocities, and hence the acoustic impedance of the nano-composite films increase with the alumina content, which gives us another option of tailoring the acoustic impedance of the nano-composite film for making the matching layer of high-frequency medical ultrasonic transducers. PMID:17375816

  2. Next Generation Hole Injection/Transport Nano-Composites for High Efficiency OLED Development

    SciTech Connect

    King Wang

    2009-07-31

    The objective of this program is to use a novel nano-composite material system for the OLED anode coating/hole transport layer. The novel anode coating is intended to significantly increase not only hole injection/transport efficiency, but the device energy efficiency as well. Another goal of the Core Technologies Program is the optimization and scale-up of air-stable and cross-linkable novel HTL nano-composite materials synthesis and the development of low-cost, large-scale mist deposition processes for polymer OLED fabrication. This proposed technology holds the promise to substantially improve OLED energy efficiency and lifetime.

  3. Layered TiO2 :PVK nano-composite thin films for photovoltaic applications. TiO2 :PVK nano-composite thin films

    NASA Astrophysics Data System (ADS)

    Kaune, G.; Wang, W.; Metwalli, E.; Ruderer, M.; Roßner, R.; Roth, S. V.; Müller-Buschbaum, P.

    2008-05-01

    The influence of the solvent used for spin-coating on the homogeneity of poly(N-vinylcarbazole) (PVK) films is investigated. Homogenous films are obtained only by the use of toluene, solution in tetrahydrofuran (THF) and chloroform results in radially oriented inhomogeneities and films prepared by use of N-methylpyrrolidone and dimethylacetamide show particle formation during spin-coating. Layered nano-composite thin films are prepared by spin-coating a PVK film on top of a nano-structured titanium dioxide ( TiO2 layer. The TiO2 thin films are prepared by a sol-gel process using an amphiphilic copolymer as structure-directing agent. Structural characterisation of the TiO2 :PVK nano-composite films is done by field emission scanning electron microscopy (FESEM) and grazing-incidence small-angle scattering (GISAXS). Bare TiO2 films are probed for comparison. Light is basically only absorbed in the ultraviolet regime and absorption slightly increases upon addition of PVK, which makes the layered TiO2 :PVK nano-composite thin films good candidates for UV photovoltaic devices. Furthermore, absorption remains stable over a period of several days.

  4. Comparison of reversed-phase/cation-exchange/anion-exchange trimodal stationary phases and their use in active pharmaceutical ingredient and counterion determinations.

    PubMed

    Liu, Xiaodong; Pohl, Christopher A

    2012-04-01

    This study involved three commercial reversed-phase (RP)/anion-exchange (AEX)/cation-exchange (CEX) trimodal columns, namely Acclaim Trinity P1 (Thermo Fisher Scientific), Obelisc R (SIELC Technologies) and Scherzo SM-C18 (Imtakt). Their chromatographic properties were compared in details with respect to hydrophobicity, anion-exchange capacity, cation-exchange capacity, and selectivity, by studying retention behavior dependency on organic solvent, buffer concentration and pH. It was found that their remarkably different column chemistries resulted in distinctive chromatography properties. Trinity P1 exhibited strong anion-exchange and cation-exchange interactions but low RP retention while Scherzo SM-C18 showed strong reversed-phase retention with little cation-exchange and anion-exchange capacities. For Obelisc R, its reversed-phase capacity was weaker than Scherzo SM-C18 but slightly higher than Trinity P1, and its ion-exchange retentions were between Trinity P1 and Scherzo SM-C18. In addition, their difference in selectivity was demonstrated by examples of determining the active pharmaceutical ingredient (API) and counterion of drug products. PMID:22209548

  5. NOVEL CONTINUOUS PH/SALT GRADIENT AND PEPTIDE SCORE FOR STRONG CATION EXCHANGE CHROMATOGRAPHY IN 2D-NANO-LC/MSMS PEPTIDE IDENTIFICATION FOR PROTEOMICS

    EPA Science Inventory

    Tryptic digests of human serum albumin (HSA) and human lung epithelial cell lysates were used as test samples in a novel proteomics study. Peptides were separated and analyzed using 2D-nano-LC/MSMS with strong cation exchange (SCX) and reverse phase (RP) chromatography and contin...

  6. Kinetic Analyses of Cation Exchange Rates in Synthetic Birnessite Measured by Time- Resolved Synchrotron X-ray Diffraction

    NASA Astrophysics Data System (ADS)

    Lopano, C. L.; Heaney, P. J.; Post, J. E.; Bandstra, J.; Brantley, S. L.

    2006-05-01

    Birnessite is the most abundant and chemically important layer-structure Mn-oxide phase found in soils, desert varnishes, and ocean nodules. It also is industrially important for use in battery technology and octahedral sieves. Due to the poorly crystalline nature of natural birnessite, synthetic analogues typically have been employed in studies that explore the structural response of birnessite to variations in interlayer composition. For this work, we measured changes in unit-cell parameters over time to quantify the degree of cation exchange as a function of concentration. Aqueous K+, Cs+, and Ba2+ cations at varying concentrations at pH 7 were exchanged for interlayer Na+ in synthetic birnessite (Na0.58(Mn4+1.42,Mn3+0.58)O4·1.5H2O) using a simple flow- through cell, and the exchange products were monitored via time-resolved X-ray powder diffraction at the National Synchrotron Light Source. Powder X-ray diffraction patterns were collected every 2-3 minutes. Rietveld analyses of X-ray diffraction patterns for K- and Ba-exchanged birnessite revealed a decrease in unit- cell volume over time. In contrast, Cs+ substitution increased cell volume. For all three cations, the crystallographic data indicate that exchange occurred in two stages. A rapid and dramatic change in unit-cell volume was followed by a modest adjustment over longer timescales. Fourier electron difference syntheses revealed that the rapid, initial stage of exchange was marked by re-configuration of the interlayer species, whereas the second, protracted phase of substitution represented ordering into the newly established interlayer positions. For the first time, we have modeled the kinetics of interlayer substitution in Na-birnessite. For purposes of comparison, we have employed a simple one-stage reaction (i.e., Na-birnessite → K-birnessite) and a two stage reaction (i.e,. Na-birnessite → K-birnessitedisordered → K- birnessiteordered). For exchange with 0.01 M KCl solutions, the single

  7. Characterization studies of plasticized PEO-PMMA nano-composite polymer electrolyte system

    NASA Astrophysics Data System (ADS)

    Sharma, Poonam; Kanchan, D. K.; Gondaliya, Nirali; Pant, Meenakshi; Jayswal, Manish S.; Joge, Prajakta

    2012-06-01

    Present study reports the characterization studies on silver based PEO-PMMA-PEG nano composite polymer electrolyte system, prepared by solution cast technique. The complexation among various constituents of polymer samples was carried by XRD and FTIR analysis. Thermal analysis of the samples was carried out by DSC study.

  8. Investigation on Dry Sliding Wear Behavior of Nylon66/GnP Nano-composite

    NASA Astrophysics Data System (ADS)

    Sankara Narayana, Kota; Suman, Koka Naga Sai; Arun Vikram, Kothapalli

    2016-06-01

    The tribological behavior of graphene nano platelets (GnP) reinforced Nylon66 polymer Nano composites were studied using a pin-on-disc apparatus under dry sliding conditions. The influence of wear control factors like applied load, velocity, sliding distance and weight percentage of GnP reinforcement on the responses like specific wear rate and frictional coefficient were investigated. Nano composites were developed by melt mixing of various weight fractions of GnP (0/0.5/1/2) with nylon 66 using twin screw extruder. A design of experiments based on the Taguchi technique was performed to acquire data in a controlled way and was successfully used to identify the optimal combinations of control factors influencing the outputs. Analysis of variance was employed to investigate the influence and contribution of control factors on the responses. The results showed that the inclusion of GnP as reinforcing material in Nylon66 Nano composites, decreases the friction coefficient and increases the wear resistance of the Nano composites significantly.

  9. Separation of Cinchona alkaloids on a novel strong cation-exchange-type chiral stationary phase-comparison with commercially available strong cation exchanger and reversed-phase packing materials.

    PubMed

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

    2009-02-01

    A recently reported chiral strong cation exchanger (cSCX) type stationary phase was investigated for the LC separation of a series of Cinchona alkaloids and synthetic derivatives thereof to test its usefulness as alternative methodology for the separation of those important pharmaceuticals. The cSCX column-packing material was qualitatively compared on the one hand against a commercially available non-enantioselective SCX-material, PolySulfoethyl-A, and, on the other hand, against a modern C18 reversed-phase stationary phase which is commonly employed for Cinchona alkaloid analysis. Both SCX columns showed no pronounced peak-tailing phenomena which typically hamper Cinchona alkaloid RP analysis and require specific optimization. Thus, the cSCX-based assay provided new feasibilities for the separation of the Cinchona alkaloids in polar organic mode as opposed to conventional reversed-phase methodologies. In particular, a method for the simultaneous determination of eight Cinchona alkaloids (quinine, quinidine, cinchonine, cinchonidine, and their corresponding dihydro analogs) using the cSCX column in HPLC has been developed and exemplarily applied to impurity profiling of a commercial alkaloid sample. Furthermore, both SCX materials allowed successful separation of C9-epi and 10,11-didehydro derivatives from their respective educts in an application in synthetic Cinchona alkaloid chemistry. PMID:19107468

  10. Mechanism of cation exchange process for epitaxy of superconducting mercury barium calcium copper oxide films and passive microwave devices

    NASA Astrophysics Data System (ADS)

    Zhao, Hua

    The record high superconducting transition temperature (T c) in Hg-based High temperature superconducting (HTS) cuprates make them very promising for both fundamental physics and practical applications. The high volatile nature of Hg presents a major challenge in epitaxy of high quality Hg-based HTS films. In a novel cation exchange process developed by our group recently, epitaxial HgBa2CaCu2O6+delta (Hg-1212) films can be obtained by diffusing volatile Tl cations out of, and simultaneously diffusing Hg cations into, the lattice of epitaxial Tl2Ba2CaCu2O8 (Tl-2212) or TlBa 2CaCu2O7 (Tl-1212) precursor films. Aiming at the remained issues in understanding the mechanism of the cation exchange (CE) process, this thesis work has studied the reversibility of CE. We have found that the CE process is completely reversible between Hg-1212 and Tl-2212, confirming further the thermal perturbation diffusion model. One of the experimental works unveiled that the conversion from Hg-1212 to Tl-2212 involves two steps: conversion from Hg-1212 to Tl-1212 via CE followed by Tl intercalation to form double Tl--O plans in each unit cell. Two improvements have been made in raising the quality of the Hg-1212 films. First, by successfully introducing micro-channels in Tl-1212 precursor with reversible CE, purer HTS Hg-1212 thin films have been obtained. Secondly, by pinning lattice with nonvolatile Re atoms, the surface morphology of Hg-1212 films have been improved. In addition to making the high quality Hg-1212 films, we have fabricated a two-pole X-band Hg-1212 microstrip filter and then investigated its nonlinearity by measuring the third-order intermodulation (IM3) signals since the major limitation for real application still comes from the nonlinearity. By a comparison between different structural materials of Hg-1212, Tl-2212 and YBa2Cu3O7 (YBCO), the third-order intercept (IP3) of the Hg-1212 filter is consistently higher than that in the YBCO and Tl-2212. The surprising

  11. Nanostructured biocompatible thermal/electrical stimuli-responsive biopolymer-doped polypyrrole for controlled release of chlorpromazine: kinetics studies.

    PubMed

    Shamaeli, Ehsan; Alizadeh, Naader

    2014-09-10

    Biocompatible nanostructured conductive heparin-doped polypyrrole film was fabricated and employed as a high-capacity cation exchanger for programmable release of neuroleptic drug, chlorpromazine (CPZ) with thermally and electrical dual-stimulation. Releasing behavior were studied at different applied potentials and temperatures by in-situ monitoring of UV absorbance measurements. Three mathematical models (Higuchi, Power, and Avrami equation) were employed to investigate kinetics of the release. Based on the obtained results, the Avrami model found to be more comprehensive than two other ones for mathematical description of electro-stimulated release of CPZ. A quantitative relationship between activation energy parameters (Ea, ΔG(≠), ΔH(≠), and ΔS(≠)) and release conditions (applied potential and temperature) has been developed and established to predict release rate constants at various applied conditions. PMID:24969668

  12. The transfer behavior of different ions across anion and cation exchange membranes under vanadium flow battery medium

    NASA Astrophysics Data System (ADS)

    Sun, Jiawei; Li, Xianfeng; Xi, Xiaoli; Lai, Qinzhi; Liu, Tao; Zhang, Huamin

    2014-12-01

    The transfer behavior of different ions (V2+, V3+, VO2+, VO2+, H+, SO42-) across ion exchange membranes is investigated under vanadium flow battery (VFB) operating condition. VX-20 anion exchange membrane (AEM) and Nafion 115 cation exchange membrane (CEM) are selected to investigate the influence of fixed charged groups on the transfer behavior of different ions. The interaction between different ions and water is discussed in detail aiming to ascertain the variation of different ions in the charge-discharge process. Under the VFB medium, the transfer behavior and function of different ions are very different for the AEM and CEM. V2+ ions at the negative side accumulate when VFB is assembled with Nafion 115, while the VO2+ ions at the positive side accumulate for VX-20. The SO42- ions will transfer across Nafion 115 to balance the charges and the protons can balance the charges of VX-20. Finally the capacity fade mechanism of different membranes is investigated, showing that the capacity decay of VFB assembled with Nafion 115 mainly results from the cross mix of vanadium ions across the membrane, however, for VX-20, the side reactions can be the major reason. This paper provides important information about electrolyte for the application of VFB.

  13. Enhanced photocatalytic activity of chromium(VI) reduction and EDTA oxidization by photoelectrocatalysis combining cationic exchange membrane processes.

    PubMed

    Hsu, Hung-Te; Chen, Shiao-Shing; Tang, Yi-Fang; Hsi, Hsing-Cheng

    2013-03-15

    A novel technology of photoelectrocatalysis (PEC) combining with cationic exchange membrane (CEM) was proposed for simultaneous reduction of chromium(VI) and oxidization of EDTA. The application of CEM was used to enhance the efficiency for prevention of the re-oxidation of reduced chromium with the electron-hole pairs. In this study, effects of current density, pH, TiO2 dosage, hydraulic retention time (HRT), light intensity and EDTA/Cr(VI) molar ratio were all investigated. The results showed that the optimum conversion efficiency occurred at 4mA/cm(2) with the presence of CEM. Higher conversion efficiencies were observed at lower pH due to the electrostatic attractions between positive charged TiOH2(+), and negatively charged Cr(VI) and EDTA. The optimum TiO2 loading of 1g/L was depended mainly on the acidic pH range, especially at higher HRT and irradiation intensity. In addition, higher EDTA/Cr(VI) molar ratio enhanced the reduction efficiency of Cr(VI), indicating EDTA plays the role of hole scavenger in this system. Moreover, incomplete EDTA decomposition contributes to the occurrence of intermediates, including nitrilotriacetic acid, iminodiacetic acid, glycine, oxamic acid, lyoxylic acid, oxalic acid, acetic acid and formic acid, as identified by GC/MS. Consequently, transformation pathway was determined from these analyzed byproducts and molecular orbital package analysis. PMID:23380448

  14. Cation exchange capacity (Qv) estimation in shaly sand reservoirs: case studies in the Junggar Basin, northwest China

    NASA Astrophysics Data System (ADS)

    Wang, Liang; Mao, Zhi-Qiang; Sun, Zhong-Chun; Luo, Xing-Ping; Deng, Ren-Shuang; Zhang, Ya-Hui; Ren, Bing

    2015-10-01

    Cation exchange capacity (Qv) is a key parameter in resistivity-based water saturation models of shaly sand reservoirs, and the accuracy of Qv calculation is crucial to the prediction of saturations of oil and gas. In this study, a theoretical expression of Qv in terms of shaly sand permeability (Kshaly-sand), total porosity (ϕt), and salinity of formation water (S) is deduced based on the capillary tube model and the physics volume model. Meanwhile, the classical Schlumberger-Doll research (SDR) model has been introduced to estimate Kshaly-sand. On this basis, a novel technique to estimate Qv from nuclear magnetic resonance (NMR) logs is proposed, and the corresponding model is also established, whose model parameters are calibrated by laboratory Qv and NMR measurements of 15 core samples from the Toutunhe formation of the Junggar Basin, northwest China. Based on the experimental data sets, this technique can be extended to reservoir conditions to estimate continuous Qv along the intervals. The processing results of field examples illustrate that the Qv calculated from field NMR logs are consistent with the analyzed results, with the absolute errors within the scope of  ±0.1 mmol cm-3 for the majority of core samples.

  15. Selective separation and purification of highly polar basic compounds using a silica-based strong cation exchange stationary phase.

    PubMed

    Long, Zhen; Guo, Zhimou; Xue, Xingya; Zhang, Xiuli; Nordahl, Lilly; Liang, Xinmiao

    2013-12-01

    Compared to moderately and weakly hydrophilic bases, highly polar basic compounds are even more difficult to separate due to their poor retention in reversed phase (RP) mode. This study described the successful applications of a strong cation exchange (SCX) stationary phase to achieve symmetric peak shape, adequate retention and selectivity in the separation of very polar basic compounds. Salt and acetonitrile concentrations were adjusted to optimize the separation. Good correlations (R(2)=0.998-1.000) between the logarithm of the retention factor and the logarithm of salt or acetonitrile concentration were obtained. Gradients generated by changing salt or acetonitrile concentration were compared for the analysis of different highly polar bases. Although all of the analytes were eluted more quickly with an acetonitrile gradient, the effect of the gradients tested on peak width and peak shape varied with respect to analyte. In addition, the effects of different types of cation and anion additives were also investigated. After separation parameters were acquired, the SCX-based method was utilized to analyze highly hydrophilic alkaloids from Scopolia tangutica Maxim with high separation efficiency (plate numbers>32,000 m(-1)). Concurrently, one very polar alkaloid fraction was purified with symmetric peak shape using the current method. Our results suggest that SCX stationary phase can be used as an alternative to RP stationary phase in the analysis and purification of highly hydrophilic basic compounds. PMID:24267097

  16. Simultaneous determination of cation exchange capacity and surface area of acid activated bentonite powders by methylene blue sorption

    NASA Astrophysics Data System (ADS)

    Yener, Nilgün; Biçer, Cengiz; Önal, Müşerref; Sarıkaya, Yüksel

    2012-01-01

    To distinguish the ion exchanged and physically adsorbed methylene blue cations (MB+) on ionic surfaces, acid activated bentonite samples were used as porous adsorbents. A natural calcium bentonite (CaB) sample from Enez/Edirne, Turkey, was acid activated at 90 °C for 16 h with various HCl/CaB ratios. The irreversible exchange and physical adsorption of MB+ cations on the ionic solids have simultaneously occurred. The ion exchanged (mex) and physically adsorbed (mad) MB+ contents were obtained as the values of sorption capacity at c = 0 and the increase to a plateaus of adsorption isotherms, respectively. The mad value was taken to be monolayer adsorption capacity. Cation exchange capacity (CEC) and specific surface area (SMB) for each sample were calculated from the mex and mad values, respectively. Also, the BET specific surface areas (SBET) and pore size distribution were determined from low temperature nitrogen adsorption/desorption data. A linear correlation between the SMB and SBET values was found.

  17. Nitrogen and chemical oxygen demand removal from septic tank wastewater in subsurface flow constructed wetlands: substrate (cation exchange capacity) effects.

    PubMed

    Collison, Robert S; Grismer, Mark E

    2014-04-01

    The current article focuses on chemical oxygen demand (COD) and nitrogen (ammonium and nitrate) removal performance from synthetic human wastewater as affected by different substrate rocks having a range of porosities and cation exchange capacities (CECs). The aggregates included lava rock, lightweight expanded shale, meta-basalt (control), and zeolite. The first three had CECs of 1 to 4 mequiv/100 gm, whereas the zeolite CEC was much greater (-80 mequiv/100 gm). Synthetic wastewater was gravity fed to each constructed wetland system, resulting in a 4-day retention time. Effluent samples were collected, and COD and nitrogen species concentrations measured regularly during four time periods from November 2008 through June 2009. Chemical oxygen demand and nitrogen removal fractions were not significantly different between the field and laboratory constructed wetland systems when corrected for temperature. Similarly, overall COD and nitrogen removal fractions were practically the same for the aggregate substrates. The important difference between aggregate effects was the zeolite's ammonia removal process, which was primarily by adsorption. The resulting single-stage nitrogen removal process may be an alternative to nitrification and denitrification that may realize significant cost savings in practice. PMID:24851327

  18. On-line cation exchange for suppression of adduct formation in negative-ion electrospray mass spectrometry of nucleic acids.

    PubMed

    Huber, C G; Buchmeiser, M R

    1998-12-15

    One major difficulty in the analysis of nucleic acids by electrospray mass spectrometry is represented by the affinity of the polyanionic sugar-phosphate backbone for nonvolatile cations, especially ubiquitous sodium and potassium ions. A simple on-line sample preparation system comprising a microflow pumping system and 45 x 0.8-mm-i.d. microcolumns packed with weak or strong cation-exchange resins is described for the efficient removal of cations from nucleic acid samples. Samples were analyzed by flow injection analysis at a 3-5 microL/min flow of 10 mM triethylamine in 50% water-50% acetonitrile. After on-line desalting, mass spectra of oligonucleotides revealed no significant sodium adduct peaks. Moreover, signal-to-noise ratios were greatly enhanced compared to direct injection of the samples. Electrospray mass spectrometry with on-line sample preparation allowed accurate molecular mass determinations of picomole amounts of crude oligonucleotide preparations ranging in size from 8 to 80 nucleotides within a few minutes. The good linearity of the calibration plot (R2 = 0.9988) over at least 2 orders of magnitude and a relative standard deviation in peak areas of less than 9% permitted the sensitive quantitative measurement of oligonucleotides in a concentration range of 0.2-20 microM with selected-ion monitoring. Finally, the on-line sample preparation system was evaluated for the mass spectrometric analysis of complex oligonucleotide mixtures. PMID:9868919

  19. Cation exchange and CaCO 3 dissolution during artificial recharge of effluent to a calcareous sandstone aquifer

    NASA Astrophysics Data System (ADS)

    Goren, Orly; Gavrieli, Ittai; Burg, Avihu; Lazar, Boaz

    2011-03-01

    SummaryThis research describes a field study and laboratory simulations of the geochemical evolution of groundwater following a recharge of effluent into aquifers. The study was conducted in the soil aquifer treatment (SAT) system of the Shafdan sewage reclamation plant, Israel. The SAT system recharges secondary effluent into the calcareous sandstone sediments of the Israeli Coastal Aquifer as a tertiary treatment. The reclaimed effluent is recovered ca. 500 m off the recharge basin and is used for unlimited irrigation. The laboratory simulations in which effluent was pumped through experimental columns packed with pristine Shafdan sediment showed that the chemical composition of the outflowing water was controlled mainly by cation exchange and CaCO 3 dissolution. Na +, K + and Mg 2+ were adsorbed and Ca 2+ was desorbed during the initial stage of recharge. The equilibrium distribution of the adsorbed cations was: Ca 2+ ˜ 60%, Mg 2+ ˜ 20%, and Na + and K + ˜ 10% each. The Ca 2+ in the Shafdan production wells and in the experimental columns outflow (˜5 meq L -1) was always higher than the Ca 2+ in the recharged effluent (˜3.5 meq L -1), indicating continuous CaCO 3 dissolution. This study demonstrates that besides mixing, a suite of geochemical processes should be considered when assessing groundwater quality following artificial recharge of aquifers.

  20. A continuous process for biodiesel production in a fixed bed reactor packed with cation-exchange resin as heterogeneous catalyst.

    PubMed

    Feng, Yaohui; Zhang, Aiqing; Li, Jianxin; He, Benqiao

    2011-02-01

    Continuous esterification of free fatty acids (FFA) from acidified oil with methanol was carried out with NKC-9 cation-exchange resin in a fixed bed reactor with an internal diameter of 25 mm and a height of 450 mm to produce biodiesel. The results showed that the FFA conversion increased with increases in methanol/oil mass ratio, reaction temperature and catalyst bed height, whereas decreased with increases in initial water content in feedstock and feed flow rate. The FFA conversion kept over 98.0% during 500 h of continuous esterification processes under 2.8:1 methanol to oleic acid mass ratio, 44.0 cm catalyst bed height, 0.62 ml/min feed flow rate and 65°C reaction temperature, showing a much high conversion and operational stability. Furthermore, the loss of sulfonic acid groups from NKC-9 resin into the production was not found during continuous esterification. In sum, NKC-9 resin shows the potential commercial applications to esterification of FFA. PMID:21078550

  1. Combined Utilization of Cation Exchanger and Neutral Receptor to Volume Reduction of Alkaline Tank Waste by Separation of Sodium Salts

    SciTech Connect

    Levitskaia, Tatiana G.; Lumetta, Gregg J.; Moyer, Bruce A.

    2004-03-29

    In this report, novel approaches to the selective liquid-liquid extraction separation of sodium hydroxide and sodium nitrate from high-level alkaline tank waste will be discussed. Sodium hydroxide can be successfully separated from alkaline tank-waste supernatants by weakly acidic lipophilic hydroxy compounds via a cation-exchange mechanism referred to as pseudo hydroxide extraction. In a multi-cycle process, as sodium hydroxide in the aqueous phase becomes depleted, it is helpful to have a neutral sodium receptor in the extraction system to exploit the high nitrate concentration in the waste solution to promote sodium removal by an ion-pair extraction process. Simultaneous utilization of an ionizable organic hydroxy compound and a neutral extractant (crown ether) in an organic phase results in the synergistic enhancement of ion exchange and improved separation selectivity due to the receptor's strong and selective sodium binding. Moreover, combination of the hydroxy compound and the crown ether provides for mutually increased solubility, even in a non-polar organic solvent. Accordingly, application of Isopar{reg_sign} L, a kerosene-like alkane solvent, becomes feasible. This investigation involves examination of such dual-mechanism extraction phases for sodium extraction from simulated and actual salt cake waste solutions. Sodium salts can be regenerated upon the contact of the loaded extraction phases with water. Finally, conditions of potential extraction/strip cycling will be discussed.

  2. The use of native cation-exchange chromatography to study aggregation and phase separation of monoclonal antibodies

    PubMed Central

    Chen, Shuang; Lau, Hollis; Brodsky, Yan; Kleemann, Gerd R; Latypov, Ramil F

    2010-01-01

    This study introduces a novel analytical approach for studying aggregation and phase separation of monoclonal antibodies (mAbs). The approach is based on using analytical scale cation-exchange chromatography (CEX) for measuring the loss of soluble monomer in the case of individual and mixed protein solutions. Native CEX outperforms traditional size-exclusion chromatography in separating complex protein mixtures, offering an easy way to assess mAb aggregation propensity. Different IgG1 and IgG2 molecules were tested individually and in mixtures consisting of up to four protein molecules. Antibody aggregation was induced by four different stress factors: high temperature, low pH, addition of fatty acids, and rigorous agitation. The extent of aggregation was determined from the amount of monomeric protein remaining in solution after stress. Consequently, it was possible to address the role of specific mAb regions in antibody aggregation by co-incubating Fab and Fc fragments with their respective full-length molecules. Our results revealed that the relative contribution of Fab and Fc regions in mAb aggregation is strongly dependent on pH and the stress factor applied. In addition, the CEX-based approach was used to study reversible protein precipitation due to phase separation, which demonstrated its use for a broader range of protein–protein association phenomena. In all cases, the role of Fab and Fc was clearly dissected, providing important information for engineering more stable mAb-based therapeutics. PMID:20512972

  3. Gamma-aminobutyric acid production using immobilized glutamate decarboxylase followed by downstream processing with cation exchange chromatography.

    PubMed

    Lee, Seungwoon; Ahn, Jungoh; Kim, Yeon-Gu; Jung, Joon-Ki; Lee, Hongweon; Lee, Eun Gyo

    2013-01-01

    We have developed a gamma-aminobutyric acid (GABA) production technique using his-tag mediated immobilization of Escherichia coli-derived glutamate decarboxylase (GAD), an enzyme that catalyzes the conversion of glutamate to GABA. The GAD was obtained at 1.43 g/L from GAD-overexpressed E. coli fermentation and consisted of 59.7% monomer, 29.2% dimer and 2.3% tetramer with a 97.6% soluble form of the total GAD. The harvested GAD was immobilized to metal affinity gel with an immobilization yield of 92%. Based on an investigation of specific enzyme activity and reaction characteristics, glutamic acid (GA) was chosen over monosodium glutamate (MSG) as a substrate for immobilized GAD, resulting in conversion of 2.17 M GABA in a 1 L reactor within 100 min. The immobilized enzymes retained 58.1% of their initial activities after ten consecutive uses. By using cation exchange chromatography followed by enzymatic conversion, GABA was separated from the residual substrate and leached GAD. As a consequence, the glutamic acid was mostly removed with no detectable GAD, while 91.2% of GABA was yielded in the purification step. PMID:23322022

  4. Cation Exchange Strategy for the Encapsulation of a Photoactive CO-Releasing Organometallic Molecule into Anionic Porous Frameworks.

    PubMed

    Carmona, Francisco J; Rojas, Sara; Sánchez, Purificación; Jeremias, Hélia; Marques, Ana R; Romão, Carlos C; Choquesillo-Lazarte, Duane; Navarro, Jorge A R; Maldonado, Carmen R; Barea, Elisa

    2016-07-01

    The encapsulation of the photoactive, nontoxic, water-soluble, and air-stable cationic CORM [Mn(tacn)(CO)3]Br (tacn = 1,4,7-triazacyclononane) in different inorganic porous matrixes, namely, the metalorganic framework bio-MOF-1, (NH2(CH3)2)2[Zn8(adeninate)4(BPDC)6]·8DMF·11H2O (BPDC = 4,4'-biphenyldicarboxylate), and the functionalized mesoporous silicas MCM-41-SO3H and SBA-15-SO3H, is achieved by a cation exchange strategy. The CO release from these loaded materials, under simulated physiological conditions, is triggered by visible light. The results show that the silica matrixes, which are unaltered under physiological conditions, slow the kinetics of CO release, allowing a more controlled CO supply. In contrast, bio-MOF-1 instability leads to the complete leaching of the CORM. Nevertheless, the degradation of the MOF matrix gives rise to an enhanced CO release rate, which is related to the presence of free adenine in the solution. PMID:27291890

  5. Analyte-Size-Dependent Ionization and Quantification of Monosaccharides in Human Plasma Using Cation-Exchanged Smectite Layers.

    PubMed

    Ding, Yuqi; Kawakita, Kento; Xu, Jiawei; Akiyama, Kazuhiko; Fujino, Tatsuya

    2015-08-01

    Smectite, a synthetic inorganic polymer with a saponite structure, was subjected to matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS). Typical organic matrix molecules 2,4,6-trihydroxyacetophenone (THAP) and 2,5-dihydroxybenzoic acid (DHBA) were intercalated into the layer spacing of cation-exchanged smectite, and the complex was used as a new matrix for laser desorption/ionization mass spectrometry. Because of layer spacing limitations, only a small analyte that could enter the layer and bind to THAP or DHBA could be ionized. This was confirmed by examining different analyte/matrix preparation methods and by measuring saccharides with different molecular sizes. Because of the homogeneous distribution of THAP molecules in the smectite layer spacing, high reproducibility of the analyte peak intensity was achieved. By using isotope-labeled (13)C6-d-glucose as the internal standard, quantitative analysis of monosaccharides in pretreated human plasma sample was performed, and the value of 8.6 ± 0.3 μg/mg was estimated. PMID:26151728

  6. Application of nano composites in the fixation and processing of histological material.

    PubMed

    Burkadze, G; Kikalishvili, N; Kargareteli, V

    2015-04-01

    The pathological examination is one of the longest in the list of medical tests. Most of this time is spent on preparation of the microslide, which involves the following phases: fixation, processing, cutting and staining. Our objective was to develop optimal regime of fixation and processing (namely, 1 and 2 stage of processing) by applying Nano composites for the development of quick, cheap and qualitative protocol of material processing. 24 various types and concentration Nano composite fixation device were used in study, made by applying single-layer, surface modified carbon nanotubes in the conditions of ultrasound treatment by UP200HT device. Also was developed Nano tubular network integration method in bio-material in the conditions of ultrasound treatment, when besides Nano composite fixation devices various Nano composite reagents (namely, 0.003% and 0.005% Nano composite alcohols) were used in material processing. There were carried out 126 experiments in sum and experiments were checked through standard processing. Fixation devices produced from formalin and alcohol base showed good result of fixation - by using them in the conditions of ultrasound treatment, practically 24 times decreased the period of fixation (as a standard of fixation was applied minimal rate of ASCO/Cap guideline dated by 2008 - 6 hours). The best way was considered Nano composite fixation device of NH2 functionalization of the 0.002% concentration on alcohol base A19 (according to the fixation rate 15 minutes with ultrasound maintenance). Nano tubular network integration method enabled us to have decreased the number of alcohols of ascending concentration and delay time in them. High time efficiency factor - Tk = 47.5% (time of new processing/ standard processing time X100) and high efficiency factor of the expense of reagents - Rk = 33% (number of reagents spent at the time of new processing/number of spent reagents at the time of standard processing X100) is obtained as a result

  7. Simultaneous determinations of Cr(VI) and Cr(III) by ion-exclusion/cation-exchange chromatography with an unmodified silica-gel column.

    PubMed

    Hirata, Shizuko; Kozaki, Daisuke; Sakanishi, Kinya; Nakagoshi, Nobukazu; Tanaka, Kazuhiko

    2010-01-01

    In order to characterize the ion-exclusion and cation-exchange properties of an unmodified silica-gel column, the retention behaviors of Cr(VI) and Cr(III) ions were investigated using a Develosil 30-5 (150 x 4.6 mm i.d.) in the acidic region. Cr(VI) was separated from other anions by an ion-exclusion and ion-adsorption mechanism, and Cr(III) was separated from other cations with a cation-exchange mechanism. When using 2.0 mM oxalic acid (pH 2.6) as an eluent, a good separation of Cr(VI) and Cr(III) was obtained using conductimetric detection in 12 min. The method was successfully applied to the simultaneous determinations of Cr(VI) and Cr(III) added into tap-water and river-water samples. PMID:20215693

  8. Application of mixed-mode, solid-phase extraction in environmental and clinical chemistry. Combining hydrogen-bonding, cation-exchange and Van der Waals interactions

    USGS Publications Warehouse

    Mills, M.S.; Thurman, E.M.; Pedersen, M.J.

    1993-01-01

    Silica- and styrene-divinylbenzene-based mixed-mode resins that contain C8, C18 and sulphonated cation-exchange groups were compared for their efficiency in isolation of neutral triazine compounds from water and of the basic drug, benzoylecgonine, from urine. The triazine compounds were isolated by a combination of Van der Waals and hydrogen-bonding interactions, and benzoylecgonine was isolated by Van der Waals interactions and cation exchange. All analytes were eluted with a polar organic solvent contaning 2% ammonium hydroxide. Larger recoveries (95%) were achieved on copolymerized mixed-mode resins where C18 and sulfonic acid are in closer proximity than on 'blended' mixed-mode resins (60-70% recovery).

  9. Novel Ultra Stable Silica-Based Stationary Phases for Reversed Phase Liquid Chromatography-Study of a Hydrophobically Assisted Weak Acid Cation Exchange Phase

    PubMed Central

    Zhang, Yu; Carr, Peter W.

    2010-01-01

    A mixed-mode reversed-phase/weak cation exchange (RP/WCX) phase has been developed by introducing a small amount of carboxylate functionality into a hydrophobic hyper-crosslinked (HC) platform. This silica based HC-platform was designed to form an extensive polystyrene network completely confined to the particle's surface. The fully connected polymer network prevents the loss of bonded phase, which leads to superior hydrolytic stability of the new phase when compared to conventional silica based phases. Compared to previously introduced HC phases the added carboxylic groups impart a new weak cation exchange selectivity to the base hydrophobic HC platform. The phase thus prepared shows a mixed-mode retention mechanism, allowing for both neutral organic compounds and bases of a wide polarity range to be simultaneously separated on the same phase under the same conditions. In addition, the new phase offers the flexibility that gradients in organic modifier, pH or ionic competitors can be used to affect the separation of a wide range of solutes. Moreover, the inherent weak acid cation exchange groups allow formic and acetic acid buffers to be used as eluents thereby avoiding the mass spectrometric ionization suppression problems concomitant to the use of non-volatile additives such as strong amine modifiers (e.g. triethylamine) or salts (e.g. NaCl) to elute basic solutes from the strong cation exchange phase which was previously developed in this lab. The use of the new phase for achieving strong retention of rather hydrophilic neurotransmitters and drugs of abuse without the need for ion pairing agents is demonstrated. PMID:21227426

  10. Absorption of artificial piggery effluent by soils: Inverse optimisation of hydraulic, solute transport, and cation exchange parameters using HP1 and UCODE

    NASA Astrophysics Data System (ADS)

    Jacques, Diederik; Smith, Chris; Simunek, Jirka; Smiles, David

    2010-05-01

    Smiles and Smith (2004) performed controlled laboratory experiments on the transport of major cations (Na, K, Mg, Ca) during water absorption in horizontal soil columns for three different times. Experimental data consists of profiles of water contents, Cl concentrations, total aqueous and sorbed concentrations of the major cations. Numerical simulation of the experimental dataset requires a coupled code that can consider variably-saturated water flow, multi-component solute transport, and geochemical reactions (aqueous complexation and cation exchange). The HP1 code, based on coupled HYDRUS-1D and PHREEQC, is used to simulate this data set. The sorption of the major cations is described as a competitive cation exchange process. The objective of the study is to calibrate hydraulic, transport, and geochemical parameters using HP1, the universal optimization code UCODE_2005 (Poeter et al., 2005), and the experimental dataset of Smiles and Smith (2004). The dataset was used to calibrate three types of parameters: soil hydraulic parameters (the parameters of the van Genuchten-Mualem model for the soil hydraulic functions), solute transport parameters (dispersivity), and geochemical parameters (exchange coefficients for the major cations and the cation exchange capacity). Different calibration runs were performed with different sets of input data, different sets of optimized parameters, and different formulations of the cation exchange process (i.e., Gapon, Rothmund-Kornfeld). Overall, the description of the dataset with the coupled code is satisfactory. Estimated parameters are within expected ranges for the type of material used. References Poeter, E.P., M.C. Hill, E.R. Banta, S. Mehl, and C. Steen, 2005. UCODE_2005 and six other computer codes for universal sensitivity analysis, calibration and uncertainty evaluation. U.S. Geological Survey Techniques and Methods 6-A11. Smiles, D.E., and C.J. Smith, 2004. Absorption of artificial piggery effluent by soil: A

  11. Ion chromatographic separation of inorganic ions using a combination of hydrophilic interaction chromatographic column and cation-exchange resin column.

    PubMed

    Arai, Kaori; Mori, Masanobu; Hironaga, Takahiro; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2012-04-01

    A combination of hydrophilic interaction chromatographic (HILIC) column and a weakly acidic cation-exchange resin (WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography (IC). Firstly, the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions. The columns used were SeQuant ZIC-HILIC (ZIC-HILIC) with a sulfobetaine-zwitterion stationary phase (ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase (HILIC-10). When using tartaric acid as the eluent, the HILIC columns indicated strong retentions for anions, based on ion-pair interaction. Especially, HILIC-10 could strongly retain anions compared with ZIC-HILIC. The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I(-) > NO3(-) > Br(-) > Cl(-) > H2PO4(-). However, since HILIC-10 could not separate analyte cations, a WCX column (TSKgel Super IC-A/C) was connected after the HILIC column in series. The combination column system of HILIC and WCX columns could successfully separate ten ions (Na+, NH4+, K+, Mg2+, Ca2+, H2PO4(-), Cl(-), Br(-), NO3(-) and I(-)) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6. The relative standard deviations (RSDs) of analyte ions by the system were in the ranges of 0.02% - 0.05% in retention times and 0.18% - 5.3% in peak areas through three-time successive injections. The limits of detection at signal-to-noise ratio of 3 were 0.24 - 0.30 micromol/L for the cations and 0.31 - 1.2 micromol/L for the anions. This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results. PMID:22799200

  12. A cation exchange model to describe Cs+ sorption at high ionic strength in subsurface sediments at Hanford site, USA.

    PubMed

    Liu, Chongxuan; Zachara, John M; Smith, Steve C

    2004-02-01

    A theoretical and experimental study of cation exchange in high ionic strength electrolytes was performed using pristine subsurface sediments from the U.S. Department of Energy Hanford site. These sediments are representative of the site contaminated sediments impacted by release of high level waste (HLW) solutions containing 137Cs+ in NaNO3 brine. The binary exchange behavior of Cs+-Na+, Cs+-K+, and Na+-K+ was measured over a range in electrolyte concentration. Vanselow selectivity coefficients (Kv) that were calculated from the experimental data using Pitzer model ion activity corrections for aqueous species showed monotonic increases with increasing electrolyte concentrations. The influence of electrolyte concentration was greater on the exchange of Na+-Cs+ than K+-Cs+, an observation consistent with the differences in ion hydration energy of the exchanging cations. A previously developed two-site ion exchange model [Geochimica et Cosmochimica Acta 66 (2002) 193] was modified to include solvent (water) activity changes in the exchanger phase through application of the Gibbs-Duhem equation. This water activity-corrected model well described the ionic strength effect on binary Cs+ exchange, and was extended to the ternary exchange system of Cs+-Na+-K+ on the pristine sediment. The model was also used to predict 137Cs+ distribution between sediment and aqueous phase (Kd) beneath a leaked HLW tank in Hanfordd's S-SX tank using the analytical aqueous data from the field and the binary ion exchange coefficients for the pristine sediment. The Kd predictions closely followed the trend in the field data and were improved by consideration of water activity effects that were considerable in certain regions of the vadose zone plume. PMID:14734247

  13. A cation exchange model to describe Cs + sorption at high ionic strength in subsurface sediments at Hanford site, USA

    NASA Astrophysics Data System (ADS)

    Liu, Chongxuan; Zachara, John M.; Smith, Steve C.

    2004-02-01

    A theoretical and experimental study of cation exchange in high ionic strength electrolytes was performed using pristine subsurface sediments from the U.S. Department of Energy Hanford site. These sediments are representative of the site contaminated sediments impacted by release of high level waste (HLW) solutions containing 137Cs + in NaNO 3 brine. The binary exchange behavior of Cs +-Na +, Cs +-K +, and Na +-K + was measured over a range in electrolyte concentration. Vanselow selectivity coefficients ( Kv) that were calculated from the experimental data using Pitzer model ion activity corrections for aqueous species showed monotonic increases with increasing electrolyte concentrations. The influence of electrolyte concentration was greater on the exchange of Na +-Cs + than K +-Cs +, an observation consistent with the differences in ion hydration energy of the exchanging cations. A previously developed two-site ion exchange model [Geochimica et Cosmochimica Acta 66 (2002) 193] was modified to include solvent (water) activity changes in the exchanger phase through application of the Gibbs-Duhem equation. This water activity-corrected model well described the ionic strength effect on binary Cs + exchange, and was extended to the ternary exchange system of Cs +-Na +-K + on the pristine sediment. The model was also used to predict 137Cs + distribution between sediment and aqueous phase ( Kd) beneath a leaked HLW tank in Hanfordd's S-SX tank using the analytical aqueous data from the field and the binary ion exchange coefficients for the pristine sediment. The Kd predictions closely followed the trend in the field data and were improved by consideration of water activity effects that were considerable in certain regions of the vadose zone plume.

  14. Tuning Equilibrium Compositions in Colloidal Cd1-xMnxSe Nanocrystals Using Diffusion Doping and Cation Exchange.

    PubMed

    Barrows, Charles J; Chakraborty, Pradip; Kornowske, Lindsey M; Gamelin, Daniel R

    2016-01-26

    The physical properties of semiconductor nanocrystals can be tuned dramatically via composition control. Here, we report a detailed investigation of the synthesis of high-quality colloidal Cd1-xMnxSe nanocrystals by diffusion doping of preformed CdSe nanocrystals. Until recently, Cd1-xMnxSe nanocrystals proved elusive because of kinetic incompatibilities between Mn(2+) and Cd(2+) chemistries. Diffusion doping allows Cd1-xMnxSe nanocrystals to be prepared under thermodynamic rather than kinetic control, allowing access to broader composition ranges. We now investigate this chemistry as a model system for understanding the characteristics of nanocrystal diffusion doping more deeply. From the present work, a Se(2-)-limited reaction regime is identified, in which Mn(2+) diffusion into CdSe nanocrystals is gated by added Se(2-), and equilibrium compositions are proportional to the amount of added Se(2-). At large added Se(2-) concentrations, a solubility-limited regime is also identified, in which x = xmax = ∼0.31, independent of the amount of added Se(2-). We further demonstrate that Mn(2+) in-diffusion can be reversed by cation exchange with Cd(2+) under exactly the same reaction conditions, purifying Cd1-xMnxSe nanocrystals back to CdSe nanocrystals with fine tunability. These chemistries offer exceptional composition control in Cd1-xMnxSe NCs, providing opportunities for fundamental studies of impurity diffusion in nanocrystals and for development of compositionally tuned nanocrystals with diverse applications ranging from solar energy conversion to spin-based photonics. PMID:26643033

  15. The effect of geometrical presentation of multimodal cation-exchange ligands on selective recognition of hydrophobic regions on protein surfaces.

    PubMed

    Woo, James; Parimal, Siddharth; Brown, Matthew R; Heden, Ryan; Cramer, Steven M

    2015-09-18

    The effects of spatial organization of hydrophobic and charged moieties on multimodal (MM) cation-exchange ligands were examined by studying protein retention behavior on two commercial chromatographic media, Capto™ MMC and Nuvia™ cPrime™. Proteins with extended regions of surface-exposed aliphatic residues were found to have enhanced retention on the Capto MMC system as compared to the Nuvia cPrime resin. The results further indicated that while the Nuvia cPrime ligand had a strong preference for interactions with aromatic groups, the Capto MMC ligand appeared to interact with both aliphatic and aromatic clusters on the protein surfaces. These observations were formalized into a new set of protein surface property descriptors, which quantified the local distribution of electrostatic and hydrophobic potentials as well as distinguishing between aromatic and aliphatic properties. Using these descriptors, high-performing quantitative structure-activity relationship (QSAR) models (R(2)>0.88) were generated for both the Capto MMC and Nuvia cPrime datasets at pH 5 and pH 6. Descriptors of electrostatic properties were generally common across the four models; however both Capto MMC models included descriptors that quantified regions of aliphatic-based hydrophobicity in addition to aromatic descriptors. Retention was generally reduced by lowering the ligand densities on both MM resins. Notably, elution order was largely unaffected by the change in surface density, but smaller and more aliphatic proteins tended to be more affected by this drop in ligand density. This suggests that modulating the exposure, shape and density of the hydrophobic moieties in multimodal chromatographic systems can alter the preference for surface exposed aliphatic or aromatic residues, thus providing an additional dimension for modulating the selectivity of MM protein separation systems. PMID:26292626

  16. Estimation of soil cation exchange capacity using Genetic Expression Programming (GEP) and Multivariate Adaptive Regression Splines (MARS)

    NASA Astrophysics Data System (ADS)

    Emamgolizadeh, S.; Bateni, S. M.; Shahsavani, D.; Ashrafi, T.; Ghorbani, H.

    2015-10-01

    The soil cation exchange capacity (CEC) is one of the main soil chemical properties, which is required in various fields such as environmental and agricultural engineering as well as soil science. In situ measurement of CEC is time consuming and costly. Hence, numerous studies have used traditional regression-based techniques to estimate CEC from more easily measurable soil parameters (e.g., soil texture, organic matter (OM), and pH). However, these models may not be able to adequately capture the complex and highly nonlinear relationship between CEC and its influential soil variables. In this study, Genetic Expression Programming (GEP) and Multivariate Adaptive Regression Splines (MARS) were employed to estimate CEC from more readily measurable soil physical and chemical variables (e.g., OM, clay, and pH) by developing functional relations. The GEP- and MARS-based functional relations were tested at two field sites in Iran. Results showed that GEP and MARS can provide reliable estimates of CEC. Also, it was found that the MARS model (with root-mean-square-error (RMSE) of 0.318 Cmol+ kg-1 and correlation coefficient (R2) of 0.864) generated slightly better results than the GEP model (with RMSE of 0.270 Cmol+ kg-1 and R2 of 0.807). The performance of GEP and MARS models was compared with two existing approaches, namely artificial neural network (ANN) and multiple linear regression (MLR). The comparison indicated that MARS and GEP outperformed the MLP model, but they did not perform as good as ANN. Finally, a sensitivity analysis was conducted to determine the most and the least influential variables affecting CEC. It was found that OM and pH have the most and least significant effect on CEC, respectively.

  17. A facile route to synthesize CdZnSe core–shell-like alloyed quantum dots via cation exchange reaction in aqueous system

    SciTech Connect

    Sheng, Yingzhuo; Wei, Jumeng; Liu, Bitao; Peng, Lingling

    2014-09-15

    Highlights: • Water-soluble CdZnSe alloyed QDs synthesized by cation exchange reaction. • The as-prepared CdZnSe QDs have fairly good luminescence properties. • The surface defects of obtained QDs were removed due to the alloyed structure. - Abstract: Water-soluble CdZnSe alloyed nanocrystals have been successfully prepared via “green” cation exchange reaction in aqueous system. The X-ray diffraction (XRD) patterns indicate that the as-prepared nanocrystals had high crystallinity and small particle size of 4–5 nm. The absorption spectra of CdZnSe show red shift of 100 nm from 375 to 475 nm. Moreover, the band-gap photoluminescent (PL) emission has a red shift of 50 nm from 430 to 480 nm with the increase of the reaction time. On the basis of the PL properties and transmission electron microscopy (TEM) images, one kind of core–shell-like structure model was proposed, which resulted from the different cation exchange reaction rates. This structure could greatly improve the luminescence properties by the removal of surface defect of quantum dots. This work would support potential applications in optoelectronic devices, and biomedical tags fields.

  18. Development of high-productivity, strong cation-exchange adsorbers for protein capture by graft polymerization from membranes with different pore sizes

    PubMed Central

    Chenette, Heather C.S.; Robinson, Julie R.; Hobley, Eboni; Husson, Scott M.

    2012-01-01

    This paper describes the surface modification of macroporous membranes using ATRP (atom transfer radical polymerization) to create cation-exchange adsorbers with high protein binding capacity at high product throughput. The work is motivated by the need for a more economical and rapid capture step in downstream processing of protein therapeutics. Membranes with three reported nominal pore sizes (0.2, 0.45, 1.0 μm) were modified with poly(3-sulfopropyl methacrylate, potassium salt) tentacles, to create a high density of protein binding sites. A special formulation was used in which the monomer was protected by a crown ether to enable surface-initiated ATRP of this cationic polyelectrolyte. Success with modification was supported by chemical analysis using Fourier-transform infrared spectroscopy and indirectly by measurement of pure water flux as a function of polymerization time. Uniformity of modification within the membranes was visualized with confocal laser scanning microscopy. Static and dynamic binding capacities were measured using lysozyme protein to allow comparisons with reported performance data for commercial cation-exchange materials. Dynamic binding capacities were measured for flow rates ranging from 13 to 109 column volumes (CV)/min. Results show that this unique ATRP formulation can be used to fabricate cation-exchange membrane adsorbers with dynamic binding capacities as high as 70 mg/mL at a throughput of 100 CV/min and unprecedented productivity of 300 mg/mL/min. PMID:23175597

  19. Fabrication of Nano-Composite Surface Layers on Aluminium Employing Friction Stir Processing Technique

    NASA Astrophysics Data System (ADS)

    Bozorg, S. F. K.; Zarghani, A. S.; Zarei-Hanzaki, A.

    2010-03-01

    Al/Al2O3 nano-composite surface layer was fabricated via friction stir processing technique. Commercial AA6082 aluminium alloy extruded bar and nanometric Al2O3 powder were subjected to friction stir processing at a substrate travel speed of 80 mm/min and a tool rotation speed of 1000 rpm using a hardened H-13 tool steel. The grain structure and reinforcement particles were investigated by using optical and scanning electron microscopy. Results show that Al2O3 particles can be more uniformly dispread in aluminium substrate by increasing the number of processing passes. Also, hardness enhancement of the nano-composite surface layer was found. This is attributed to uniform dispersion of Al2O3 particles.

  20. Two-Step SPD Processing of a Trimodal Al-Based Nano-Composite

    NASA Astrophysics Data System (ADS)

    Zhang, Yuzheng; Sabbaghianrad, Shima; Yang, Hanry; Topping, Troy D.; Langdon, Terence G.; Lavernia, Enrique J.; Schoenung, Julie M.; Nutt, Steven R.

    2015-12-01

    An ultrafine-grained (UFG) aluminum nano-composite was fabricated using two severe plastic deformation steps: cryomilling of powders (and subsequent consolidation of blended powders by forging) followed by high-pressure torsion (HPT). The forged bulk composite featured a trimodal structure comprised of UFG, coarse grain (CG) regions, and ceramic particles. The additional HPT processing introduced finer grain sizes and altered the morphology and spatial distribution of the ductile CG regions. As a result, both strength and ductility increased substantially compared to those of the Al nano-composite prior to HPT. The increases were attributed to the more optimal shape and spacing of the CG regions which promoted uniform elongation and yielding during tensile loading. Microstructural changes were characterized at each processing step to establish the evolution of microstructure and to elucidate structure-property relationships. The toughening effect of the CG regions was documented via fracture analysis, providing a potential strategy for designing microstructures with enhanced strength and toughness.

  1. Fabrication of Nano-Composite Surface Layers on Aluminium Employing Friction Stir Processing Technique

    SciTech Connect

    Bozorg, S. F. K.; Zarghani, A. S.; Zarei-Hanzaki, A.

    2010-03-11

    Al/Al{sub 2}O{sub 3} nano-composite surface layer was fabricated via friction stir processing technique. Commercial AA6082 aluminium alloy extruded bar and nanometric Al{sub 2}O{sub 3} powder were subjected to friction stir processing at a substrate travel speed of 80 mm/min and a tool rotation speed of 1000 rpm using a hardened H-13 tool steel. The grain structure and reinforcement particles were investigated by using optical and scanning electron microscopy. Results show that Al{sub 2}O{sub 3} particles can be more uniformly dispread in aluminium substrate by increasing the number of processing passes. Also, hardness enhancement of the nano-composite surface layer was found. This is attributed to uniform dispersion of Al{sub 2}O{sub 3} particles.

  2. Fabrication of TI/SIC Surface Nano-Composite Layer by Friction Stir Processing

    NASA Astrophysics Data System (ADS)

    Shamsipur, Ali; Kashani-Bozorg, Seyed Farshid; Zareie-Hanzaki, Abbas

    In the present investigation, novel Ti/SiC surface nano-composite layer was successfully fabricated by dispersing nano-sized SiC particles into commercially pure titanium plates employing friction stir processing technique. The process parameters such as tool rotation and advancing speeds were adjusted to produce defect-free surface composite layer, however, uniform distribution of the nano-size SiC particles in a matrix of titanium was achieved after the second pass. The micro hardness value of the Ti/SiC nano-composite surface layer was found to be 534 HV; this is 3.3 times higher than that of the commercially pure titanium substrate. No reaction was detected between SiC powders and the titanium matrix after friction stir processing.

  3. Finite Element Model Characterization Of Nano-Composite Thermal And Environmental Barrier Coatings

    NASA Technical Reports Server (NTRS)

    Yamada, Yoshiki; Zhu, Dongming

    2011-01-01

    Thermal and environmental barrier coatings have been applied for protecting Si based ceramic matrix composite components from high temperature environment in advanced gas turbine engines. It has been found that the delamination and lifetime of T/EBC systems generally depend on the initiation and propagation of surface cracks induced by the axial mechanical load in addition to severe thermal loads. In order to prevent T/EBC systems from surface cracking and subsequent delamination due to mechanical and thermal stresses, T/EBC systems reinforced with nano-composite architectures have showed promise to improve mechanical properties and provide a potential crack shielding mechanism such as crack bridging. In this study, a finite element model (FEM) was established to understand the potential beneficial effects of nano-composites systems such as SiC nanotube-reinforced oxide T/EBC systems.

  4. Synthesis of NiMnO3/C nano-composite electrode materials for electrochemical capacitors

    NASA Astrophysics Data System (ADS)

    Kakvand, Pejman; Safi Rahmanifar, Mohammad; El-Kady, Maher F.; Pendashteh, Afshin; Kiani, Mohammad Ali; Hashami, Masumeh; Najafi, Mohsen; Abbasi, Ali; Mousavi, Mir F.; Kaner, Richard B.

    2016-08-01

    Demand for high-performance energy storage materials has motivated research activities to develop nano-engineered composites that benefit from both high-rate and high-capacitance materials. Herein, NiMnO3 (NMO) nanoparticles have been synthesized through a facile co-precipitation method. As-prepared NMO samples are then employed for the synthesis of nano-composites with graphite (Gr) and reduced graphene oxide (RGO). Various samples, including pure NMO, NMO-graphite blend, as well as NMO/Gr and NMO/RGO nano-composites have been electrochemically investigated as active materials in supercapacitors. The NMO/RGO sample exhibited a high specific capacitance of 285 F g‑1 at a current density of 1 A g‑1, much higher than the other samples (237 F g‑1 for NMO/Gr, 170 F g‑1 for NMO-Gr and 70 F g‑1 for NMO). Moreover, the NMO/RGO nano-composite has shown excellent cycle stability with a 93.5% capacitance retention over 1000 cycles at 2 A g‑1 and still delivered around 87% of its initial capacitance after cycling for 4000 cycles. An NMO/RGO composite was assessed in practical applications by assembling NMO/RGO//NMO/RGO symmetric devices, exhibiting high specific energy (27.3 Wh kg‑1), high specific power (7.5 kW kg‑1), and good cycle stability over a broad working voltage of 1.5 V. All the obtained results demonstrate the promise of NMO/RGO nano-composite as a high-performance electrode material for supercapacitors.

  5. Synthesis of NiMnO3/C nano-composite electrode materials for electrochemical capacitors.

    PubMed

    Kakvand, Pejman; Rahmanifar, Mohammad Safi; El-Kady, Maher F; Pendashteh, Afshin; Kiani, Mohammad Ali; Hashami, Masumeh; Najafi, Mohsen; Abbasi, Ali; Mousavi, Mir F; Kaner, Richard B

    2016-08-01

    Demand for high-performance energy storage materials has motivated research activities to develop nano-engineered composites that benefit from both high-rate and high-capacitance materials. Herein, NiMnO3 (NMO) nanoparticles have been synthesized through a facile co-precipitation method. As-prepared NMO samples are then employed for the synthesis of nano-composites with graphite (Gr) and reduced graphene oxide (RGO). Various samples, including pure NMO, NMO-graphite blend, as well as NMO/Gr and NMO/RGO nano-composites have been electrochemically investigated as active materials in supercapacitors. The NMO/RGO sample exhibited a high specific capacitance of 285 F g(-1) at a current density of 1 A g(-1), much higher than the other samples (237 F g(-1) for NMO/Gr, 170 F g(-1) for NMO-Gr and 70 F g(-1) for NMO). Moreover, the NMO/RGO nano-composite has shown excellent cycle stability with a 93.5% capacitance retention over 1000 cycles at 2 A g(-1) and still delivered around 87% of its initial capacitance after cycling for 4000 cycles. An NMO/RGO composite was assessed in practical applications by assembling NMO/RGO//NMO/RGO symmetric devices, exhibiting high specific energy (27.3 Wh kg(-1)), high specific power (7.5 kW kg(-1)), and good cycle stability over a broad working voltage of 1.5 V. All the obtained results demonstrate the promise of NMO/RGO nano-composite as a high-performance electrode material for supercapacitors. PMID:27324723

  6. Marginal and internal fit of nano-composite CAD/CAM restorations

    PubMed Central

    Park, So-Hyun; Shin, Yoo-Jin

    2016-01-01

    Objectives The purpose of this study was to compare the marginal and internal fit of nano-composite CAD-CAM restorations. Materials and Methods A full veneer crown and an mesio-occluso-distal (MOD) inlay cavity, which were prepared on extracted human molars, were used as templates of epoxy resin replicas. The prepared teeth were scanned and CAD-CAM restorations were milled using Lava Ultimate (LU) and experimental nano-composite CAD/CAM blocks (EB) under the same milling parameters. To assess the marginal and internal fit, the restorations were cemented to replicas and were embedded in an acrylic mold for sectioning at 0.5 mm intervals. The measured gap data were pooled according to the block types and measuring points for statistical analysis. Results Both the block type and measuring point significantly affected gap values, and their interaction was significant (p = 0.000). In crowns and inlays made from the two blocks, gap values were significantly larger in the occlusal area than in the axial area, while gap values in the marginal area were smallest (p < 0.001). Among the blocks, the restorations milled from EB had a significantly larger gap at all measuring points than those milled from LU (p = 0.000). Conclusions The marginal and internal gaps of the two nano-composite CAD/CAM blocks differed according to the measuring points. Among the internal area of the two nano-composite CAD/CAM restorations, occlusal gap data were significantly larger than axial gap data. The EB crowns and inlays had significantly larger gaps than LU restorations. PMID:26877989

  7. Growth, Morphology, and Electrical Characterization of Polyaniline-ZnO Nano-composite Langmuir-Blodgett Thin Films

    NASA Astrophysics Data System (ADS)

    Bhullar, Gurpreet Kaur; Kaur, Ramneek; Raina, K. K.

    2015-10-01

    Polyaniline (PANi)-zinc oxide (ZnO) nano-composites were prepared by chemical polymerization of aniline doped with ZnO nanoparticles. Surface pressure-area ( π-A) isotherms for the PANi-ZnO nano-composite revealed phase transformations of the monolayer during compression. Langmuir-Blodgett (LB) films of PANi and PANi-ZnO nano-composite were characterized by use of UV-visible (UV-Vis) and Fourier-transform infrared spectroscopy, atomic force microscopy, and conductive atomic force microscopy (C-AFM). Local current-voltage ( I- V) characteristics revealed the current range for PANi-ZnO nano-composite LB films was larger than that for PANi LB films. Conductive data images were recorded to investigate charge-transport current inhomogeneities in the LB films.

  8. Acrylic coatings exhibiting improved hardness, solvent resistance and glossiness by using silica nano-composites

    NASA Astrophysics Data System (ADS)

    Dashtizadeh, Ahmad; Abdouss, Majid; Mahdavi, Hossein; Khorassani, Manuchehr

    2011-01-01

    To prepare nano-composite emulsion acrylic resins with improved surface hardness and solvent resistance, nano-silica particles were treated with surfactants. The monomers of methyl methacrylate/butylacrylate were co-polymerized on the surface of dispersed silica particles. Several emulsions with different silica contents and copolymer mole fractions were prepared. Finally the emulsions were modified to water-based acrylic coatings and improved properties such as surface hardness, solvent resistance and glossiness were determined. The study of coatings was directed to find the improved resin by optimum surface properties. Size distribution and morphology of latexes were characterized by Fourier transform infrared spectroscopy, dynamic light scattering, transmission electron microscopy and scanning electron microscopy. The glass transition temperature of nano-composites was measured and discussed its relation with silica contents, monomer mole fractions and improved properties of coatings. The optimum pendulum hardness of coatings was on 0.46 methyl methacrylate mole fraction and 120 g silica content. An increase in pendulum hardness of nano-composites with the addition of modified silica was observed. DLS and TEM studies indicate that silica particles were dispersed homogenously through the polymer matrix.

  9. Effect of interface on mechanical properties and biodegradation of PCL HAp supramolecular nano-composites.

    PubMed

    Shokrollahi, Parvin; Mehmanchi, Mohammad; Atai, Mohammad; Omidian, Hossein; Shokrolahi, Fateme

    2014-01-01

    This research explores the correlation between the structural properties of supramolecular biocomposites and their mechanical strength. Hybrid biocomposites composed of surface-modified hydroxyapatite nano-particles and supramolecular polycaprolactone (SP PCL), were prepared at different compositions, and their mechanical, thermal and viscoelastic properties as well as biodegradability, biocompatibility and cytotoxicity were evaluated in vitro. The results were compared with those for SP PCL/naked hydroxyapatite nano-composites. We show that surface modification of hydroxyapatite nanoparticles resulted in outstanding improvement of tensile strength and modulus up to 3.6 and 2.2-fold, respectively. At above 10 wt% HAp and 20 wt% HApUPy, heterogeneous nano-composites with inferior mechanical properties were obtained. Based on rheological (in steady shear mode) and small/wide angle X-ray scattering measurements, unusual improved mechanical properties were ascribed to the formation of supramolecular clusters around nanoparticles. In-vitro degradation of the supramolecular nano-composites was also studied to investigate the overall product biodegradation as well as toxicity of the degradation product(s). PMID:24030697

  10. Mechanical and barrier properties of guar gum based nano-composite films.

    PubMed

    Saurabh, Chaturbhuj K; Gupta, Sumit; Bahadur, Jitendra; Mazumder, S; Variyar, Prasad S; Sharma, Arun

    2015-06-25

    Guar gum based nano-composite films were prepared using organically modified (cloisite 20A) and unmodified (nanofil 116) nanoclays. Effect of nanoclay incorporation on mechanical strength, water vapor barrier property, chromatic characteristics and opacity of films was evaluated. Nano-composites were characterized using X-ray scattering, FTIR and scanning electron microscopy. A nanoclay concentration dependent increase in mechanical strength and reduction in water vapor transmission rate was observed. Films containing nanofil 116 (2.5% w/w guar gum) and closite 20A (10% w/w guar gum) demonstrated a 102% and 41% higher tensile strength, respectively, as compared to the control. Lower tensile strength of cloisite 20A films as compared to nanofil 116 films was due to its incompatibility with guar gum. X-ray scattering analysis revealed that interstitial spacing between nanofil 116 and cloisite 20A sheets increased due to intercalation by guar gum polymer. This resulted in improved mechanical and barrier properties of nano-composites compared to control. PMID:25839796

  11. Coulometric differential FFT admittance voltammetry determination of Amlodipine in pharmaceutical formulation by nano-composite electrode.

    PubMed

    Norouzi, Parviz; Gupta, Vinod Kumar; Larijani, Bagher; Rasoolipour, Solmaz; Faridbod, Farnoush; Ganjali, Mohammad R

    2015-01-01

    An electrochemical detection technique based on combination of was coulometric differential fast Fourier transformation admittance voltammetry (CDFFTAV) and nano-composite film modified glassy carbon electrode was successfully applied for sensitive determination of Amlodipine. The nano-composite film was made by a mixture of ionic liquid, 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIMBF4), multiwall carbon nanotube and Au nanoparticles as electrochemical mediators. Studies reveal that the irreversible oxidation of Amlodipine was highly facile on the electrode surface. The electrochemical response was established on calculation of the charge under the admittance peak, which was obtained by discrete integration of the admittance response in a selected potential range, obtained in a flow injection analysis. Once established the best operative optimum conditions, the resulting nano-composite film electrode showed a catalytic effect on the oxidation of the analyte. The response is linear in the Amlodipine concentration range of 1.0 × 10(-9) to 2.0 × 10(-7)M with a detection limit of 1.25 × 10(-10)M. Moreover, the proposed technique exhibited high sensitivity, fast response time (less than 6s) and long-term stability and reproducibility around 96%, and it was successfully used to the determination of Amlodipine content in the pharmaceutical formulation. PMID:25281143

  12. Combined cation-exchange and extraction chromatographic method of pre-concentration and concomitant separation of Cu(II) with high molecular mass liquid cation exchanger after its online detection.

    PubMed

    Mandal, B; Roy, U S; Datta, D; Ghosh, N

    2011-08-19

    A selective method has been developed for the extraction chromatographic trace level separation of Cu(II) with Versatic 10 (liquid cation exchanger) coated on silanised silica gel (SSG-V10). Cu(II) has been extracted from 0.1M acetate buffer at the range of pH 4.0-5.5. The effects of foreign ions, pH, flow-rate, stripping agents on extraction and elution have been investigated. Exchange capacity of the prepared exchanger at different temperatures with respect to Cu(II) has been determined. The extraction equilibrium constant (K(ex)) and different standard thermodynamic parameters have also been calculated by temperature variation method. Positive value of ΔH (7.98 kJ mol⁻¹) and ΔS (0.1916 kJ mol⁻¹) and negative value of ΔG (-49.16 kJ mol⁻¹) indicated that the process was endothermic, entropy gaining and spontaneous. Preconcentration factor was optimized at 74.7 ± 0.2 and the desorption constants K(desorption)¹(1.4 × 10⁻²) and K(desorption)²(9.8 × 10⁻²) were determined. The effect of pH on R(f) values in ion exchange paper chromatography has been investigated. In order to investigate the sorption isotherm, two equilibrium models, the Freundlich and Langmuir isotherms, were analyzed. Cu(II) has been separated from synthetic binary and multi-component mixtures containing various metal ions associated with it in ores and alloy samples. The method effectively permits sequential separation of Cu(II) from synthetic quaternary mixture containing its congeners Bi(III), Sn(II), Hg(II) and Cu(II), Cd(II), Pb(II) of same analytical group. The method was found effective for the selective detection, removal and recovery of Cu(II) from industrial waste and standard alloy samples following its preconcentration on the column. A plausible mechanism for the extraction of Cu(II) has been suggested. PMID:21764063

  13. Improvement in biocompatibility of ZrO2-Al2O3 nano-composite by addition of HA.

    PubMed

    Kong, Young-Min; Bae, Chang-Jun; Lee, Su-Hee; Kim, Hae-Won; Kim, Hyoun-Ee

    2005-02-01

    The biocompatibility of zirconia-alumina (ZA) nano-composites in load-bearing applications such as dental/orthopedic implants was significantly enhanced by the addition of bioactive HA. The ZA matrix was composed of nano-composite powder obtained from the Pechini process and had higher flexural strength than conventionally mixed zirconia-alumina composite. Because the ZA nano-composite powder effectively decreased the contact area between HA and zirconia for their reaction during the sintering process, the HA-added ZA nano-composites contained biphasic calcium phosphates (BCP) of HA/TCP and had higher flexural strength than conventionally mixed ZA-HA composite. From the in vitro test with osteoblastic cell-lines, the proliferation and the differentiation (as expressed by the alkaline phosphatase activity) of the cellular response on the HA-added ZA nano-composites gradually increased as the amount of HA added increased. From the mechanical and biological evaluations of the HA-added ZA nano-composites, 30HA (30 vol% HA + 70 vol% ZA) was found to be the optimal composition for load-bearing biological applications. PMID:15276359

  14. Insights in understanding aggregate formation and dissociation in cation exchange chromatography for a structurally unstable Fc-fusion protein.

    PubMed

    Chen, Zhiqiang; Huang, Chao; Chennamsetty, Naresh; Xu, Xuankuo; Li, Zheng Jian

    2016-08-19

    Cation-exchange chromatography (CEX) of a structurally unstable Fc-fusion protein exhibited multi-peak elution profile upon a salt-step elution due to protein aggregation during intra-column buffer transition where low pH and high salt coexisted. The protein exhibited a single-peak elution behavior during a pH-step elution; nevertheless, the levels of soluble aggregates (i.e. high molecular weight species, HMW) in the CEX eluate were still found up to 12-fold higher than that for the load material. The amount of the aggregates formed upon the pH-step elution was dependent on column loading with maximum HMW achieved at intermediate loading levels, supporting the hypothesis that the aggregation was the result of both the conformational changes of the bound protein and the solution concentration of the aggregation-susceptible proteins during elution. Factors such as high load pH, short protein/resin contact time, hydrophilic resin surface, and weak ionizable ligand were effective, to some extent, to reduce aggregate formation by improving the structural integrity of the bound protein. An orthogonal technique, differential scanning fluorimetry (DSF) using Sypro Orange dye confirmed that the bound protein exposed more hydrophobic area than the native molecule in free solution, especially in the pH 4-5 range. The Sypro Orange dye study of resin surface property also demonstrated that the poly[styrene-divinylbenzene]-based Poros XS with polyhydroxyl surface coating is more hydrophobic compared to the agarose-based CM Sepharose FF and SP Sepharose FF. The hydrophobic property of Poros XS contributed to stronger interactions with the partially unfolded bound protein and consequently to the higher aggregate levels seen in Poros XS eluate. This work also investigates the aggregation reversibility in CEX eluate where up to 66% of the aggregates were observed to dissociate into native monomers over a period of 120h, and links the aggregate stability to such conditions as resin

  15. Unfolding and aggregation of monoclonal antibodies on cation exchange columns: effects of resin type, load buffer, and protein stability.

    PubMed

    Guo, Jing; Carta, Giorgio

    2015-04-01

    The chromatographic behavior of a monoclonal antibody (mAb) that exhibits a pronounced two-peak elution behavior is studied for a range of strong cation exchange resins and with varying load buffer pH and composition. Six stationary phases are considered, including two tentacle-type resins (Fractogel EMD SO3-(M) and Eshmuno S), a resin with grafted polymeric surface extenders (Nuvia S), a resin with a bimodal pore size distribution (POROS HS 50), and two macroporous resins without polymer grafts (Source 30S and UNOsphere Rapid S). The two-peak elution behavior is very pronounced for the tentacle and polymer-grafted resins and for POROS HS 50, but is essentially absent for the two macroporous resins. The extent of this behavior decreases as the buffer pH and concentration increase and, consequently, mAb binding becomes weaker. Replacing sodium with arginine as the buffer counterion, which is expected to decrease the mAb binding strength, nearly completely eliminates the two-peak behavior, while replacing sodium with tetra-n-butylammonium hydroxide, which is expected to increase the mAb binding strength, dramatically exacerbate the effect. As shown by hydrogen-deuterium exchange mass spectrometry (HX-MS), the two-peak elution behavior is related to conformational changes that occur when the mAb binds. These changes result in increased solvent exposure of specific peptides in the Fc-region for either the Fractogel or the Nuvia resin. No significant conformational changes were seen by HX-MS when the mAb was bound to the UNOsphere resin or on the Fractogel resin when arginine was used in lieu of sodium as the load buffer counterion. Experiments with two additional mAbs on the Fractogel resin show that the two-peak elution behavior is dependent on the particular antibody. Circular dichroism suggests that the propensity of different mAbs to either precipitate directly or to form stabilizing intermolecular structures upon exposure to thermal stress can be related to their

  16. Suitability of the methylene blue test for determination of cation exchange capacity of clay minerals related to ammonium acetate method

    NASA Astrophysics Data System (ADS)

    Milošević, Maja; Logar, Mihovil; Dojčinović, Biljana; Erić, Suzana

    2015-04-01

    Cation exchange capacity (CEC) represents one of the most important parameters of clay minerals which reflects their ability to exchange cations with liquid phases in near contact. Measurement of CEC is used for characterizing sample plasticity, adsorbing and swelling properties which later define their usage in industrial purposes. Several methods have been developed over the years for determination of layer charge, charge density, charge distribution, etc. and have been published in numerous papers (Czimerova et al., 2006; Yukselen and Kaya, 2008). The main goal of present study is comparison of suitability of more recent method - methylene blue test in regard to older method - ammonium acetate for determination of CEC. For this study, we selected one montmorillonite clay (Bogovina, Serbia) and two mainly kaolinite clays (Miličinica, Serbia). Chemicals used for CEC determinations were solution of methylene blue (MB)(14*10-6M/ml) and ammonium acetate (AA) solution (1M). The obtained results are showing generally lower values in case of MB method. The main difference is due to molecular aggregation of MB on the clay surface. AA method is highly sensitive to the presence of CaO. Release of Ca ion from the sample into the solution can limit the saturation of exchange sites by the ammonium ion. This is clearly visible in case of montmorillonite clay. Fe2+ and Mg ions are difficult to move by the ammonium ion because of their ion radius, but in case of MB molecule there is no such restriction in removing them from the exchange sites. MB solution, even in a low concentration (2*10-6M/ml), is showing preferable results in moving the ions from their positions which is already visible after adding a small quantity of solution (25cm3). Both MB-titration and MB-spot test yield similar results and are much simpler methods than AA and they also give other information such as specific surface area (external and internal) whereas AA method only provides information about

  17. Near-Infrared Emitting CuInSe₂/CuInS₂ Dot Core/Rod Shell Heteronanorods by Sequential Cation Exchange.

    PubMed

    van der Stam, Ward; Bladt, Eva; Rabouw, Freddy T; Bals, Sara; Donega, Celso de Mello

    2015-11-24

    The direct synthesis of heteronanocrystals (HNCs) combining different ternary semiconductors is challenging and has not yet been successful. Here, we report a sequential topotactic cation exchange (CE) pathway that yields CuInSe2/CuInS2 dot core/rod shell nanorods with near-infrared luminescence. In our approach, the Cu(+) extraction rate is coupled to the In(3+) incorporation rate by the use of a stoichiometric trioctylphosphine-InCl3 complex, which fulfills the roles of both In-source and Cu-extracting agent. In this way, Cu(+) ions can be extracted by trioctylphosphine ligands only when the In-P bond is broken. This results in readily available In(3+) ions at the same surface site from which the Cu(+) is extracted, making the process a direct place exchange reaction and shifting the overall energy balance in favor of the CE. Consequently, controlled cation exchange can occur even in large and anisotropic heterostructured nanocrystals with preservation of the size, shape, and heterostructuring of the template NCs into the product NCs. The cation exchange is self-limited, stopping when the ternary core/shell CuInSe2/CuInS2 composition is reached. The method is very versatile, successfully yielding a variety of luminescent CuInX2 (X = S, Se, and Te) quantum dots, nanorods, and HNCs, by using Cd-chalcogenide NCs and HNCs as templates. The approach reported here thus opens up routes toward materials with unprecedented properties, which would otherwise remain inaccessible. PMID:26449673

  18. Effect of cation-exchange pretreatment of aqueous soil extracts on the gas chromatographic-mass spectrometric determination of nerve agent hydrolysis products after tert.-butyldimethylsilylation.

    PubMed

    Kataoka, M; Tsunoda, N; Ohta, H; Tsuge, K; Takesako, H; Seto, Y

    1998-10-23

    The efficiency of pretreatment of aqueous soil extracts using a cation-exchange resin has been investigated by gas chromatographic-mass spectrometric (GC-MS) determination of nerve agent hydrolysis products after tert.-butyldimethylsilyl (TBDMS) derivatization. An aqueous solution containing methylphosphonic acid (MPA) and its monoalkyl esters, ethyl methylphosphonic acid, isopropyl methylphosphonic acid and pinacolyl methylphosphonic acid, was dried, and these phosphonic acids were derivatized with N-methyl-N-(tert.-butyldimethylsilyl)trifluoro-acetamide and analyzed by GC-MS. The yields of TBDMS derivatives were significantly decreased by the addition of calcium and magnesium ions to an aqueous solution (approximately 0.5 mM) before derivatization. The extent of lowered yields was related to the hydrophilicity of phosphonic acids. MPA and its monoalkyl esters were spiked into soil samples (sand, alluvial soil and volcanic ash soil), extracted with distilled water, dried, silylated and applied to GC-MS. The yields of TBDMS derivatives of monoalkyl esters from soil samples were low (3-42%) and MPA derivative was scarcely detected (yield: < 0.7%). By desalting the aqueous soil extract by passage through a strong cation-exchange resin, the yields of TBDMS derivatives of monoalkyl esters were significantly improved (12-69%) and MPA derivative was detected (yield: 2-36%). The extent of improved yields was related to the concentrations of divalent metal cations in aqueous soil extracts. In combination with desalting by the cation-exchange resin, GC-MS after TBDMS derivatization enables detection of nerve agent hydrolysis products in soils at sub-ppm (0.2 microgram/g) concentrations. PMID:9818434

  19. Near-Infrared Emitting CuInSe2/CuInS2 Dot Core/Rod Shell Heteronanorods by Sequential Cation Exchange

    PubMed Central

    2015-01-01

    The direct synthesis of heteronanocrystals (HNCs) combining different ternary semiconductors is challenging and has not yet been successful. Here, we report a sequential topotactic cation exchange (CE) pathway that yields CuInSe2/CuInS2 dot core/rod shell nanorods with near-infrared luminescence. In our approach, the Cu+ extraction rate is coupled to the In3+ incorporation rate by the use of a stoichiometric trioctylphosphine-InCl3 complex, which fulfills the roles of both In-source and Cu-extracting agent. In this way, Cu+ ions can be extracted by trioctylphosphine ligands only when the In–P bond is broken. This results in readily available In3+ ions at the same surface site from which the Cu+ is extracted, making the process a direct place exchange reaction and shifting the overall energy balance in favor of the CE. Consequently, controlled cation exchange can occur even in large and anisotropic heterostructured nanocrystals with preservation of the size, shape, and heterostructuring of the template NCs into the product NCs. The cation exchange is self-limited, stopping when the ternary core/shell CuInSe2/CuInS2 composition is reached. The method is very versatile, successfully yielding a variety of luminescent CuInX2 (X = S, Se, and Te) quantum dots, nanorods, and HNCs, by using Cd-chalcogenide NCs and HNCs as templates. The approach reported here thus opens up routes toward materials with unprecedented properties, which would otherwise remain inaccessible. PMID:26449673

  20. Formation of gypsum and bassanite by cation exchange reactions in the absence of free-liquid H2O: Implications for Mars

    NASA Astrophysics Data System (ADS)

    Wilson, Siobhan A.; Bish, David L.

    2011-09-01

    Smectites and hydrated Mg sulfate minerals have been identified in close association at various locations on the Martian surface. The hydration states of sulfates and smectites are dependent on temperature and relative humidity (RH), and therefore these minerals have the potential to affect cycling and bioavailability of H2O on Mars. We have conducted X-ray powder diffraction experiments to investigate cycling of H2O within mixtures of Ca-bearing smectites and hydrated Mg sulfate minerals under conditions of varying RH similar to those that exist at or just beneath the Martian surface. Our experiments show that under conditions of varying RH, cation-exchange reactions occur between these two potential components of the Martian regolith, producing gypsum [CaSO4·2H2O] and bassanite [CaSO4·˜0.5H2O] in the absence of free-liquid H2O. Cation-exchange reactions were accompanied by significant loss of porosity, warping of the sample surface and, in some cases, volume expansion. The formation of Ca sulfate minerals in these experiments provides evidence for the development of thin films of H2O at mineral surfaces and suggests that similar processes may operate at the arid surface of Mars. Humidity-driven cation-exchange reactions between smectites and hydrated Mg sulfate minerals may therefore play a role in shaping the present-day Martian surface and could have provided a transient source of H2O and nutrients (e.g., major and trace elements and possibly organic micro/macronutrients) for putative microorganisms.

  1. Photocatalytic studies of Ho–Zr–O nano-composite with controllable composition and defects

    SciTech Connect

    Du, Weimin; Zhao, Guoyan; Chang, Hongxun; Shi, Fei; Zhu, Zhaoqiang; Qian, Xuefeng

    2013-09-15

    With the help of sol–gel method assisted by melting salt, a series of Ho–Zr–O nano-composite with controllable composition and defects have been successfully prepared. Characterization results show that the positions, intensity, and width of the X-ray diffraction peaks of the products have a regular variation with the increase of zirconium element which implies the gradual changes of crystal spacing and product size. At the same time, the molar ratios between holmium and zirconium ions are consistent with the chemical formula and both of them are uniformly distributed in products further showing the perfect formation of targeted materials. Optical properties reveal that diversified defect forms of Ho–Zr–O nano-composite lead to the different absorptions of visible light. Photocatalytic experiments demonstrate Zr{sub 0.8}Ho{sub 0.2}O{sub 2−δ} nano-crystals have excellent visible-light-responsive photocatalytic activities on some familiar dyes (e.g.: methylene blue and Rhodamine B) which results from the special defect structure, better absorption of visible light and larger specific surface area. It follows that Zr{sub 0.8}Ho{sub 0.2}O{sub 2−δ} nano-crystals are a new kind of visible-light-responsive photocatalysts with better prospects in conversion and utilization of solar energy. Also, the present melting salt assisted route might be generalized to synthesize other AxByOz composite oxide nano-crystals with more complicated structures. - Highlights: • Ho–Zr–O nano-composite with controllable composition and defects has been obtained. • Diversified defect forms of products lead to the different visible light absorption. • Zr{sub 0.8}Ho{sub 0.2}O{sub 2−δ} nano-crystals have excellent photocatalytic activities.

  2. Electrochemical Synthesis of Graphene/MnO2 Nano-Composite for Application to Supercapacitor Electrode.

    PubMed

    Jeong, Kwang Ho; Lee, Hyeon Jeong; Simpson, Michael F; Jeong, Mun

    2016-05-01

    Graphene/MnO2 nano-composite was electrochemically synthesized for application to an electrode material for electrochemical supercapacitors. The nanosized needle-like MnO2 was obtained by use of a graphene substrate. The prepared composite exhibited an ideal supercapacitive behavior. A capacitance retention of 94% was achieved with a 4 h deposition time (an initial capacitance of 574 mF/cm2 at a scan rate of 20 mV/s) and the retention declined with further deposition time. The results demonstrate enhanced contact between the electrode and electrolyte and improved power density as an electrochemical capacitor. PMID:27483800

  3. Digital laser printing of metal/metal-oxide nano-composites with tunable electrical properties.

    PubMed

    Zenou, M; Sa'ar, A; Kotler, Z

    2016-01-01

    We study the electrical properties of aluminum structures printed by the laser forward transfer of molten, femtoliter droplets in air. The resulting printed material is an aluminum/aluminum-oxide nano-composite. By controlling the printing conditions, and thereby the droplet volume, its jetting velocity and duration, it is possible to tune the electrical resistivity to a large extent. The material resistivity depends on the degree of oxidation which takes place during jetting and on the formation of electrical contact points as molten droplets impact the substrate. Evidence for these processes is provided by FIB cross sections of printed structures. PMID:26606150

  4. Plasma Sprayed Si Nano Composite Powders for Negative Electrode of Lithium Ion Batteries

    NASA Astrophysics Data System (ADS)

    Kaga, Mashiro; Hideshima, Tasuku; Kambara, Makoto

    The electrochemical performance of the Si nano composite powders produced by PS-PVD was analyzed with Li counter electrode. The PS-PVD powders have showed an improved capacity compared to the raw mg-Si as negative electrode. Furthermore composite powders produced with CH4 addition showed higher specific gravimetric capacities per Si active materials of 1200 mAh/g, compared to 1024 mAh/g for the powders without C, suggesting the effectiveness of C coating on to the primary nano-Si and SiC particle inclusion for reinforcement of the active materials.

  5. Digital laser printing of metal/metal-oxide nano-composites with tunable electrical properties

    NASA Astrophysics Data System (ADS)

    Zenou, M.; Sa'ar, A.; Kotler, Z.

    2016-01-01

    We study the electrical properties of aluminum structures printed by the laser forward transfer of molten, femtoliter droplets in air. The resulting printed material is an aluminum/aluminum-oxide nano-composite. By controlling the printing conditions, and thereby the droplet volume, its jetting velocity and duration, it is possible to tune the electrical resistivity to a large extent. The material resistivity depends on the degree of oxidation which takes place during jetting and on the formation of electrical contact points as molten droplets impact the substrate. Evidence for these processes is provided by FIB cross sections of printed structures.

  6. Study of rheological, viscoelastic and vulcanization behavior of sponge EPDM/NR blended nano- composites

    NASA Astrophysics Data System (ADS)

    Arshad Bashir, M.; Shahid, M.; Ahmed, Riaz; Yahya, A. G.

    2014-06-01

    In this research paper the effect of blending ratio of natural rubber (NR) with Ethylene Propylene Diene Monomer (EPDM) were investigated. Different samples of EPDM/NR ratio were prepared to study the variation of NR in EPDM on rheology, curing characteristics, tangent δ, and viscosity variation during vulcanization of sponge nano composites.The main aim of present research is to develop elastomeric based sponge composites with the blending ratio of base elastomers along with the carbon nano particles for high energy absorbing and damping applications. The curing characteristics, rheology and viscoelastic nature of the composite is remarkably influenced with the progressive blending ratio of the base elastomeric matrix.

  7. Ion-exclusion chromatography with conductimetric detection of aliphatic carboxylic acids on a weakly acidic cation-exchange resin by elution with benzoic acid-beta-cyclodextrin.

    PubMed

    Tanaka, Kazuhiko; Mori, Masanobu; Xu, Qun; Helaleh, Murad I H; Ikedo, Mikaru; Taoda, Hiroshi; Hu, Wenzhi; Hasebe, Kiyoshi; Fritz, James S; Haddad, Paul R

    2003-05-16

    In this study, an aqueous solution consisting of benzoic acid with low background conductivity and beta-cyclodextrin (beta-CD) of hydrophilic nature and the inclusion effect to benzoic acid were used as eluent for the ion-exclusion chromatographic separation of aliphatic carboxylic acids with different pKa values and hydrophobicity on a polymethacrylate-based weakly acidic cation-exchange resin in the H+ form. With increasing concentration of beta-cyclodextrin in the eluent, the retention times of the carboxylic acids decreased due to the increased hydrophilicity of the polymethacrylate-based cation-exchange resin surface from the adsorption of OH groups of beta-cyclodextrin. Moreover, the eluent background conductivity decreased with increasing concentration of beta-cyclodextrin in 1 mM benzoic acid, which could result in higher sensitivity for conductimetric detection. The ion-exclusion chromatographic separation of carboxylic acids with high resolution and sensitivity was accomplished successfully by elution with a 1 mM benzoic acid-10 mM cyclodextrin solution without chemical suppression. PMID:12830884

  8. Determination of some aliphatic carboxylic acids in anaerobic digestion process waters by ion-exclusion chromatography with conductimetric detection on a weakly acidic cation-exchange resin column.

    PubMed

    Ito, Kazuaki; Takayama, Yohichi; Ikedo, Mikaru; Mori, Masanobu; Taoda, Hiroshi; Xu, Qun; Hu, Wenzhi; Sunahara, Hiroshi; Hayashi, Tsuneo; Sato, Shinji; Hirokawa, Takeshi; Tanaka, Kazuhiko

    2004-06-11

    The determination of seven aliphatic carboxylic acids, formic, acetic, propionic, isobutyric, n-butyric, isovaleric and n-valeric acids in anaerobic digestion process waters was examined using ion-exclusion chromatography with conductimetric detection. The analysis of these biologically important carboxylic acids is necessary as a measure for evaluating and controlling the process. The ion-exclusion chromatography system employed consisted of polymethacrylate-based weakly acidic cation-exchange resin columns (TSKgel OApak-A or TSKgel Super IC-A/C). weakly acidic eluent (benzoic acid), and conductimetric detection. Particle size and cation-exchange capacity were 5 microm and 0.1 meq./ml for TSKgel OApak-A and 3 microm and 0.2 meq./ml for TSKgel Super IC-A/C, respectively. A dilute eluent (1.0-2.0 mM) of benzoic acid was effective for the high resolution and highly conductimetric detection of the carboxylic acids. The good separation of isobutyric and n-butyric acids was performed using the TSKgel Super IC-A/C column (150 mm x 6.0 mm i.d. x 2). The simple and good chromatograms were obtained by the optimized ion-exclusion chromatography conditions for real samples from mesophilic anaerobic digestors, thus the aliphatic carboxylic acids were successfully determined without any interferences. PMID:15250416

  9. Cation exchange synthesis of uniform PbSe/PbS core/shell tetra-pods and their use as near-infrared photodetectors.

    PubMed

    Mishra, N; Mukherjee, B; Xing, G; Chakrabortty, S; Guchhait, A; Lim, J Y

    2016-08-01

    In this work we explore the preparation of complex-shaped semiconductor nanostructures composed of different materials via a cationic exchange process in which the cations of the original semiconductor nanostructure are replaced by cations of different metals with preservation of the shape and the anionic framework of the nanocrystals. Utilizing this cation exchange method, we synthesized two new tetrapods for the first time: Cu2-xSe/Cu2-xS and PbSe/PbS, both prepared from CdSe/CdS tetrapods as 'templates'. We also fabricated near-infrared (NIR) photodetectors with a very simple architecture comprising a PbSe/PbS tetrapod layer between two Au electrodes on a glass substrate. When illuminated by a NIR laser, these devices are capable of achieving a responsivity of 11.9 A W(-1) without the use of ligand-exchange processes, thermal annealing or hybrid device architecture. Transient absorption spectroscopy was carried out on these PbSe/PbS tetrapods, the results of which suggest that the branched morphology contributes in part to device performance. Investigation of the charge dynamics of the PbSe/PbS tetrapods revealed an extremely long-lived exciton recombination lifetime of ∼17 ms, which can result in enhanced photoconductive gain. Overall, these heterostructured tetrapods showcase simultaneously the importance of nanoparticle shape, band structure, and surface chemistry in the attainment of NIR photodetection. PMID:27387963

  10. Fabrication, characterization and photocatalytic properties of Ag/AgI/BiOI heteronanostructures supported on rectorite via a cation-exchange method

    SciTech Connect

    Chen, Yunfang; Fang, Jianzhang; Lu, Shaoyou; Wu, Yan; Chen, Dazhi; Huang, Liyan; Xu, Weicheng; Zhu, Ximiao; Fang, Zhanqiang

    2015-04-15

    Highlights: • Ag/AgI/BiOI-rectorite was prepared by twice cation-exchange process. • Ag/AgI/BiOI-rectorite photocatalyst possessed SPR and adsorption capacity. • Ag/AgI/BiOI-rectorite exhibited highly photocatalytic activity. • Trapped holes and ·O{sub 2}{sup −} were formed active species in the photocatalytic system. - Abstract: In this work, a new plasmonic photocatalyst Ag/AgI/BiOI-rectorite was prepared via a cation exchange process. The photocatalyst had been characterized by X-ray powder diffraction (XRD), Raman spectra, nitrogen sorption (BET), field-emission scanning electron microscope (FE-SEM), X-ray photoelectron spectroscopy (XPS) and UV–vis diffuse reflectance spectroscopy (DRS). The photocatalytic activity, which was evaluated by degradation of rhodamine B (RhB) and bisphenol A (BPA) under visible light irradiation, was enhanced significantly by loading Ag/AgI/BiOI nanoparticles onto rectorite. The photogenerated holes and superoxide radical (·O{sub 2}{sup −}) were both formed as active species for the photocatalytic reactions under visible light irradiation. The existence of metallic Ag particles, which possess the surface plasmon resonance effect, acted as an indispensable role in the photocatalytic reaction.

  11. Cation exchange reactions controlling desorption of Sr-90(2+) from coarse-grained contaminated sediments at the Hanford site, Washington

    SciTech Connect

    McKinley, James P.; Zachara, John M.; Smith, Steven C.; Liu, Chongxuan

    2007-01-15

    Nuclear waste that bore 90Sr2+ was accidentally leaked into the vadose zone at the Hanford site, and was immobilized at relatively shallow depths in sediments containing little apparent clay or silt-sized components. Sr2+, 90Sr2+, Mg2+, and Ca2+ was desorbed and total inorganic carbon concentration was monitored during the equilibration of this sediment with varying concentrations of Na+, Ca2+. A cation exchange model previously developed for similar sediments was applied to these results as a predictor of final solution compositions. The model included binary exchange reactions for the four operant cations and an equilibrium dissolution/precipitation reaction for calcite. The model successfully predicted the desorption data. The contaminated sediment was also examined using digital autoradiography, a sensitive tool for imaging the distribution of radioactivity. The exchanger phase containing 90Sr was found to consist of smectite formed from weathering of mesostasis glass in basaltic lithic fragments. These clasts are a significant component of Hanford formation sands. The relatively small but significant cation exchange capacity of these sediments was thus a consequence of reaction with physically sequestered clays in sediment that contained essentially no fine-grained material. The nature of this exchange component explained the relatively slow (scale of days) evolution of desorption solutions. The experimental and model results indicated that there is little risk of migration of 90Sr2+ to the water table.

  12. Cation Exchange Combined with Kirkendall Effect in the Preparation of SnTe/CdTe and CdTe/SnTe Core/Shell Nanocrystals.

    PubMed

    Jang, Youngjin; Yanover, Diana; Čapek, Richard Karel; Shapiro, Arthur; Grumbach, Nathan; Kauffmann, Yaron; Sashchiuk, Aldona; Lifshitz, Efrat

    2016-07-01

    Controlling the synthesis of narrow band gap semiconductor nanocrystals (NCs) with a high-quality surface is of prime importance for scientific and technological interests. This Letter presents facile solution-phase syntheses of SnTe NCs and their corresponding core/shell heterostructures. Here, we synthesized monodisperse and highly crystalline SnTe NCs by employing an inexpensive, nontoxic precursor, SnCl2, the reactivity of which was enhanced by adding a reducing agent, 1,2-hexadecanediol. Moreover, we developed a synthesis procedure for the formation of SnTe-based core/shell NCs by combining the cation exchange and the Kirkendall effect. The cation exchange of Sn(2+) by Cd(2+) at the surface allowed primarily the formation of SnTe/CdTe core/shell NCs. Further continuation of the reaction promoted an intensive diffusion of the Cd(2+) ions, which via the Kirkendall effect led to the formation of the inverted CdTe/SnTe core/shell NCs. PMID:27331900

  13. Enrichment and low-level determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water after cleanup by cation exchange resin.

    PubMed

    Küsters, Markus; Gerhartz, Michael

    2010-04-01

    For the determination of glyphosate, aminomethylphosphonic acid and glufosinate in drinking water, different procedures of enrichment and cleanup were examined using anion exchange or SPE. In many cases interactions of, e.g. alkaline earth metal ions especially calcium could be observed during enrichment and cleanup resulting in loss of analytes. For that reason, a novel cleanup and enrichment procedure for the determination of these phosphonic acid herbicides has been developed in drinking water using cation-exchange resin. In summary, the cleanup procedure with cation-exchange resin developed in this study avoids interactions as described above and is applicable to calcium-rich drinking water samples. After derivatization with 9-fluorenylmethylchloroformate followed by LC with fluorescence detection, LOD of 12, 14 and 12 ng/L and mean recoveries from real-world drinking water samples of 98+/-9, 100+/-16 and 101+/-11% were obtained for glyphosate, aminomethylphosphonic acid and glufosinate, respectively. The low LODs and the high precision permit the analysis of these phosphonic acid herbicides according to the guidelines of the European Commission. PMID:20183819

  14. High pressure synthesis of novel, zeolite based nano-composite materials

    NASA Astrophysics Data System (ADS)

    Santoro, M.; Gorelli, F. A.; Bini, R.; Haines, J.; Cambon, O.; Levelut, C.; van der Lee, A.; Garbarino, G.

    2014-05-01

    Zeolites exhibit an immense range of applications, such as those in the chemical industry, electronics and photonics among others. We used non-catalytic zeolites in an entirely new fashion. In fact, high pressure (0.5-26 GPa) chemical reactions of simple molecules in the pores of a pure SiO2 zeolite, silicalite were performed in the diamond anvil cell to obtain unique nano-composites with drastically modified properties. These materials were investigated using a combination of X-ray diffraction and optical spectroscopy. We will first show how silicalite can be easily filled by simple molecules at high pressures and how this filling deactivates pressure induced amorphization of the silica framework. We will then present a silicon carbonate phase synthesized by reacting silicalite and molecular CO2 that fills the nano-pores, at 18-26 GPa and 600-980 K; the resulting compound is slightly metastable at room pressure. On the other hand, a nano-composite, which is stable at room temperature and pressure, is obtained by photo-polymerizing ethylene at 0.5-1.5 GPa under UV (351-364 nm) irradiation in the channels of silicalite. The structure of this material is characterized by single polyethylene chains adapting very well to the confining channels, which significantly modifies the physical properties of the silicalite framework. These findings may pave the way to the high pressure synthesis of a unique generation of technological materials.

  15. Fabrication and characterization of the nano-composite of whey protein hydrolysate chelated with calcium.

    PubMed

    Xixi, Cai; Lina, Zhao; Shaoyun, Wang; Pingfan, Rao

    2015-03-01

    The nano-composites of whey protein hydrolysate (WPH) chelated with calcium were fabricated in aqueous solution at 30 °C for 20 min, with the ratio of hydrolysate to calcium 15 : 1 (w/w). UV scanning spectroscopy, fluorescent spectroscopy, Fourier transform infrared spectroscopy, dynamic light scattering and atomic force microscopy were applied to characterize the structure of the WPH-calcium chelate. The nano-composites showed the successful incorporation of calcium into the WPH, indicating the interaction between calcium and WPH. The chelation of calcium ions to WPH caused molecular folding and aggregation which led to the formation of a WPH-calcium chelate of nanoparticle size, and the principal sites of calcium-binding corresponded to the carboxyl groups and carbonyl groups of WPH. The WPH-calcium chelate demonstrated excellent stability and absorbability under both acidic and basic conditions, which was beneficial for calcium absorption in the gastrointestinal tract of the human body. Moreover, the calcium absorption of the WPH-calcium chelate on Caco-2 cells was significantly higher than those of calcium gluconate and CaCl₂ in vitro, suggesting the possible increase in calcium bioavailability. The findings suggest that the WPH-calcium chelate has the potential in making dietary supplements for improving bone health of the human body. PMID:25588126

  16. Micro/nano composited tungsten material and its high thermal loading behavior

    NASA Astrophysics Data System (ADS)

    Fan, Jinglian; Han, Yong; Li, Pengfei; Sun, Zhiyu; Zhou, Qiang

    2014-12-01

    Tungsten (W) is considered as promising candidate material for plasma facing components (PFCs) in future fusion reactors attributing to its many excellent properties. Current commercial pure tungsten material in accordance with the ITER specification can well fulfil the performance requirements, however, it has defects such as coarse grains, high ductile-brittle transition temperature (DBTT) and relatively low recrystallization temperature compared with its using temperature, which cannot meet the harsh wall loading requirement of future fusion reactor. Grain refinement has been reported to be effective in improving the thermophysical and mechanical properties of W. In this work, rare earth oxide (Y2O3/La2O3) and carbides (TiC/ZrC) were used as dispersion phases to refine W grains, and micro/nano composite technology with a process of 'sol gel - heterogeneous precipitation - spray drying - hydrogen reduction - ordinary consolidation sintering' was invented to introduce these second-phase particles uniformly dispersed into W grains and grain-boundaries. Via this technology, fine-grain W materials with near-full density and relatively high mechanical properties compared with traditional pure W material were manufactured. Preliminary transient high-heat flux tests were performed to evaluate the thermal response under plasma disruption conditions, and the results show that the W materials prepared by micro/nano composite technology can endure high-heat flux of 200 MW/m2 (5 ms).

  17. Long-term corrosion protection by a thin nano-composite coating

    NASA Astrophysics Data System (ADS)

    Ejenstam, Lina; Tuominen, Mikko; Haapanen, Janne; Mäkelä, Jyrki M.; Pan, Jinshan; Swerin, Agne; Claesson, Per M.

    2015-12-01

    We report and discuss the corrosion protective properties of a thin nano-composite coating system consisting of an 11 μm thick polyester acrylate (PEA) basecoat, covered by an approximately 1-2 μm thick layer of TiO2 nanoparticles carrying a 0.05 μm thick hexamethyl disiloxane (HMDSO) top coat. The corrosion protective properties were evaluated on carbon steel substrates immersed in 3 wt% NaCl solution by open circuit potential (OCP) and electrochemical impedance spectroscopy (EIS) measurements. The protective properties of each layer, and of each pair of layers, were also evaluated to gain further understanding of the long-term protective properties offered by the nano-composite coating. The full coating system showed excellent corrosion protective properties in the corrosive environment of 3 wt% NaCl-solution for an extended period of 100 days, during which the coating impedance, at the lower frequency limit (0.01 Hz), remained above 108 Ω cm2. We suggest that the excellent corrosion protective properties of the complete coating system is due to a combination of (i) good adhesion and stability of the PEA basecoat, (ii) the surface roughness and the elongated diffusion path provided by the addition of TiO2 nanoparticles, and (iii) the low surface energy provided by the HMDSO top coat.

  18. Preparation and characterization of new nano-composite scaffolds loaded with vascular stents.

    PubMed

    Xu, Hongzhen; Su, Jiansheng; Sun, Jun; Ren, Tianbin

    2012-01-01

    In this study, vascular stents were fabricated from poly (lactide-ɛ-caprolactone)/collagen/nano-hydroxyapatite (PLCL/Col/nHA) by electrospinning, and the surface morphology and breaking strength were observed or measured through scanning electron microscopy and tensile tests. The anti-clotting properties of stents were evaluated for anticoagulation surfaces modified by the electrostatic layer-by-layer self-assembly technique. In addition, nano-composite scaffolds of poly (lactic-co-glycolic acid)/polycaprolactone/nano-hydroxyapatite (PLGA/PCL/nHA) loaded with the vascular stents were prepared by thermoforming-particle leaching and their basic performance and osteogenesis were tested in vitro and in vivo. The results show that the PLCL/Col/nHA stents and PLGA/PCL/nHA nano-composite scaffolds had good surface structures, mechanical properties, biocompatibility and could guide bone regeneration. These may provide a new way to build vascularized-tissue engineered bone to repair large bone defects in bone tissue engineering. PMID:22489156

  19. Fabrication and characterization of electroless Ni-P-ZrO2 nano-composite coatings

    NASA Astrophysics Data System (ADS)

    Yang, Yongjian; Chen, Weiwei; Zhou, Chungen; Xu, Huibin; Gao, Wei

    2011-05-01

    A novel technique has been developed to produce nano-particle oxide reinforced metal coatings. This method is based on electroless deposition process by adding ZrO2 sol into conventional electroless Ni-P plating bath. Ni-P-ZrO2 nano-composite coatings have been produced with highly dispersive ZrO2 nano-particles inside the alloy coating matrix. The as plated nano-composite coating exhibits much increased microhardness up to 1045 HV200 and remarkably improved wear resistance. X-ray and electron diffraction patterns show a phase transformation in the Ni matrix of the coating from amorphous to nanocrystalline when ZrO2 sol is introduced into the coating. By comparison with the plain Ni-P coating and conventional Ni-P-ZrO2 composite coating incorporated with solid ZrO2 powders, two mechanisms for the increased mechanical properties are proposed based on nano-particle dispersion strengthening and phase transformation strengthening. The formation mechanism of ZrO2 nano-particle is also discussed.

  20. Surface modifications and Nano-composite coatings to improve the bonding strength of titanium-porcelain.

    PubMed

    Guo, Litong; Chen, Xiaoyuan; Liu, Xuemei; Feng, Wei; Li, Baoe; Lin, Cheng; Tao, Xueyu; Qiang, Yinghuai

    2016-04-01

    Surface modifications of Ti and nano-composite coatings were employed to simultaneously improve the surface roughness, corrosion resistance and chemical bonding between porclain-Ti. The specimens were studied by field-emission scanning electron microscopy, surface roughness, differential scanning calorimetry, Fourier transform infrared spectroscopy, corrosion resistance and bonding strength tests. The SEM results showed that hybrid structures with micro-stripes, nano-pores and nano-protuberances were prepared by surface modification of Ti, which significantly enhanced the surface roughness and corrosion resistance of Ti. Porous nano-composite coatings were synthesized on Ti anodized with pre-treatment in 40% HF acid. TiO2 nanoparticles were added into the hybrid coating to increase the solid phase content of the sols and avoid the formation of microcracks. With the TiO2 content increasing from 45 wt% to 60 wt%, the quantities of the microcracks on the coating surface gradually decreased. The optimal TiO2 content for the nanocomposite coatings is 60 wt% in this research. Compared to the uncoated group, the bonding strength of the coated groups showed a bonding strength improvement of 23.96%. The cytotoxicity of the 4# coating group was ranked as zero, which corresponds to non-cytotoxicity. PMID:26838834

  1. Monitoring of ppm level humic acid in surface water using ZnO-chitosan nano-composite as fluorescence probe

    NASA Astrophysics Data System (ADS)

    Basumallick, Srijita; Santra, Swadeshmukul

    2015-05-01

    Surface water contains natural pollutants humic acid (HA) and fulvic acid at ppm level which form carcinogenic chloro-compounds during chlorination in water treatment plants. We report here synthesis of ZnO-chitosan (CS) nano-composites by simple hydrothermal technique and examined their application potential as fluorescent probe for monitoring ppm level HA. These ZnO-CS composites have been characterized by HRTEM, EDX, FTIR, AFM and Fluorescence Spectra. HRTEM images show the formation of ZnO-CS nano-composites of average diameter of 50-250 nm. Aqueous dispersions of these nano-composites show fluorescence emission at 395 nm when excited at 300 nm which is strongly quenched by ppm level HA indicating their possible use in monitoring ppm level HA present in surface water.

  2. Inverter Surge Voltage Endurance with Various Surge Voltage Waveforms of Organic / Inorganic Nano-composite Enameled Wire

    NASA Astrophysics Data System (ADS)

    Kikuchi, Hideyuki; Hanawa, Hidehito

    We developed the new power supply that is able to output various kinds of surge voltage waveform and investigated partial discharge resistance of the nano-composite enameled wires using colloid solution mixing method. Experimental results revealed the relationship between surge voltage waveform and failure time of voltage endurance, as well as the difference in the strength and frequency of the partial discharge under the various kinds of surge voltage waveform. In addition, the developed nano-composite enameled wires have been verified to contribute to the improvement of the motor quality until the present time because long lifetime was confirmed in voltage endurance test with the damaged enameled wire and actual motor.

  3. Multiferroic properties of stretchable BiFeO3 nano-composite film

    NASA Astrophysics Data System (ADS)

    Hwang, J. S.; Cho, J. Y.; Park, S. Y.; Yoo, Y. J.; Yoo, P. S.; Lee, B. W.; Lee, Y. P.

    2015-02-01

    We present a simple drop-casting method for preparing multiferroic nano-composite film where BiFeO3 (BFO) nanoparticles (NPs) were evenly dispersed into polyvinyl alcohol (PVA) polymer. BFO NPs used in this work were synthesized by the conventional sol-gel method, having diameter of tens of nm and being in good crystallinity. The BFO NPs were loaded into a highly insulating PVA polymer solution as filler. The multiferroic properties of the film reveal ferromagnetic ordering due to the uncompensated spiral ordering and saturated ferroelectric curves due to the cut-off of current leakage. Moreover, the prepared films show high flexibility and their multiferroicities are preserved well even in a high curved condition, reflecting the possibility for fabricating wearable devices based on multiferroic materials.

  4. Self-Assembled Silica Nano-Composite Polymer Electrolytes: Synthesis, Rheology & Electrochemistry

    SciTech Connect

    Khan, Saad A.: Fedkiw Peter S.; Baker, Gregory L.

    2007-01-24

    The ultimate objectives of this research are to understand the principles underpinning nano-composite polymer electrolytes (CPEs) and facilitate development of novel CPEs that are low-cost, have high conductivities, large Li+ transference numbers, improved electrolyte-electrode interfacial stability, yield long cycle life, exhibit mechanical stability and are easily processable. Our approach is to use nanoparticulate silica fillers to formulate novel composite electrolytes consisting of surface-modified fumed silica nano-particles in polyethylene oxides (PEO) in the presence of lithium salts. We intend to design single-ion conducting silica nanoparticles which provide CPEs with high Li+ transference numbers. We also will develop low-Mw (molecular weight), high-Mw and crosslinked PEO electrolytes with tunable properties in terms of conductivity, transference number, interfacial stability, processability and mechanical strength

  5. Synthesis, characterization and magnetic behavior of Co/MCM-41 nano-composites

    NASA Astrophysics Data System (ADS)

    Cuello, N.; Elías, V.; Crivello, M.; Oliva, M.; Eimer, G.

    2013-09-01

    Synthesis, structure and magnetic properties of Co/MCM-41 as magnetic nano-composites have been investigated. Mesoporous materials with different degrees of metal loading were prepared by wet impregnation and characterized by ICP, XRD, N2 adsorption, UV-vis DRS, TPR and EPMA-EDS. Cobalt oxide clusters and Co3O4 nano-particles could be confined inside the mesopores of MCM-41, being this fact favored by the Co loading increasing. In addition, larger crystals of Co3O4 detectable by XRD also grow on the surface when the Co loading is enhanced. The magnetic characterization was performed in a SQUID magnetometer using a maximum magnetic applied field µ0Ha=1 T. While the samples with the higher Co loadings showed a behavior typically paramagnetic, a superparamagnetic contribution is more notorious for lower loadings, suggesting high Co species dispersion.

  6. Superconducting properties of Nb-Cu nano-composites and nano-alloys

    NASA Astrophysics Data System (ADS)

    Parab, Pradnya; Kumar, Sanjeev; Bhui, Prabhjyot; Bagwe, Vivas; Bose, Sangita

    2016-05-01

    The evolution of the superconducting transition temperature (Tc) in nano-composite and nano-alloys of Nb-Cu, grown by DC magnetron co-sputtering are investigated. Microstructure of these films depends less strongly on the ratio of Nb:Cu but more on the growth temperature. At higher growth temperature, phase separated granular films of Nb and Cu were formed which showed superconducting transition temperatures (Tc) of ~ 7.2±0.5K, irrespective of the composition. Our results show that this is primarily influenced by the microstructure of the films determined during growth which rules out the superconducting proximity effect expected in these systems. At room temperature growth, films with nano-scale alloying were obtained at the optimal compositional range of 45-70 atomic% (At%) of Nb. These were also superconducting with a Tc of 3.2K.

  7. Room temperature synthesis of high temperature stable lanthanum phosphate–yttria nano composite

    SciTech Connect

    Sankar, Sasidharan; Raj, Athira N.; Jyothi, C.K.; Warrier, K.G.K.; Padmanabhan, P.V.A.

    2012-07-15

    Graphical abstract: A facile aqueous sol–gel route involving precipitation–peptization mechanism followed by electrostatic stabilization is used for synthesizing nanocrystalline composite containing lanthanum phosphate and yttria. Highlights: ► A novel lanthanum phosphate–Y{sub 2}O{sub 3} nano composite is synthesized for the first time using a modified facile sol gel process. ► The composite becomes crystalline at 600 °C and X-ray diffraction pattern is indexed for monoclinic LaPO{sub 4} and cubic yttria. ► The composite synthesized was tested up to 1300 °C and no reaction between the phases of the constituents is observed with the morphologies of the phases being retained. -- Abstract: A facile aqueous sol–gel route involving precipitation–peptization mechanism followed by electrostatic stabilization is used for synthesizing nanocrystalline composite containing lanthanum phosphate and yttria. Lanthanum phosphate (80 wt%)–yttria (20 wt%) nano composite (LaPO{sub 4}–20%Y{sub 2}O{sub 3}), has an average particle size of ∼70 nm after heat treatment of precursor at 600 °C. TG–DTA analysis reveals that stable phase of the composite is formed on heating the precursor at 600 °C. The TEM images of the composite show rod shape morphology of LaPO{sub 4} in which yttria is acquiring near spherical shape. Phase identification of the composite as well as the phase stability up to 1300 °C was carried out using X-ray diffraction technique. With the phases being stable at higher temperatures, the composite synthesized should be a potential material for high temperature applications like thermal barrier coatings and metal melting applications.

  8. A method to buffer the concentrations of free Zn and Cd ions using a cation exchange resin in bacterial toxicity studies

    SciTech Connect

    Knight, B.; McGrath, S.P.

    1995-12-01

    The chemical form or species of metal present in a growth system is crucial to the toxicity of that metal. A growth medium is described in which the free metal concentration of either Zn or Cd is known. A method using a cation exchange resin as a buffer to maintain free metal ion concentrations during microbial growth is discussed. Using a buffered system, free concentrations of 3.4 {micro}g Cd L{sup {minus}1} and 57 {micro}g Zn L{sup {minus}1} reduced the growth rate of a sensitive isolate of Rhizobium leguminosarum biovar trifolii. The results demonstrate that to assess the true toxicity of Cd and Zn, the free ion concentration must be considered and that small free concentrations must be buffered.

  9. Selective Cation Exchange in the Core Region of Cu2–xSe/Cu2–xS Core/Shell Nanocrystals

    PubMed Central

    2015-01-01

    We studied cation exchange (CE) in core/shell Cu2–xSe/Cu2–xS nanorods with two cations, Ag+ and Hg2+, which are known to induce rapid exchange within metal chalcogenide nanocrystals (NCs) at room temperature. At the initial stage of the reaction, the guest ions diffused through the Cu2–xS shell and reached the Cu2–xSe core, replacing first Cu+ ions within the latter region. These experiments prove that CE in copper chalcogenide NCs is facilitated by the high diffusivity of guest cations in the lattice, such that they can probe the whole host structure and identify the preferred regions where to initiate the exchange. For both guest ions, CE is thermodynamically driven as it aims for the formation of the chalcogen phase characterized by the lower solubility under the specific reaction conditions. PMID:26360611

  10. High pH reversed-phase chromatography with fraction concatenation as an alternative to strong-cation exchange chromatography for two-dimensional proteomic analysis

    PubMed Central

    Yang, Feng; Shen, Yufeng; Camp, David G.; Smith, Richard D.

    2012-01-01

    Summary Orthogonal high-resolution separations are critical for attaining improved analytical dynamic range and protein coverage in proteomic measurements. High pH reversed-phase liquid chromatography (RPLC) followed by fraction concatenation affords better peptide analysis than conventional strong-cation exchange (SCX) chromatography applied for the two-dimensional proteomic analysis. For example, concatenated high pH reversed-phase liquid chromatography increased identification for peptides (1.8-fold) and proteins (1.6-fold) in shotgun proteomics analyses of a digested human protein sample. Additional advantages of high pH RPLC with fraction concatenation include improved protein sequence coverage, simplified sample processing, and reduced sample losses, making this an attractive alternative to SCX chromatography in conjunction with the second dimension low pH RPLC for two-dimensional proteomics analyses. PMID:22462785

  11. Cation exchange synthesis of uniform PbSe/PbS core/shell tetra-pods and their use as near-infrared photodetectors

    NASA Astrophysics Data System (ADS)

    Mishra, N.; Mukherjee, B.; Xing, G.; Chakrabortty, S.; Guchhait, A.; Lim, J. Y.

    2016-07-01

    In this work we explore the preparation of complex-shaped semiconductor nanostructures composed of different materials via a cationic exchange process in which the cations of the original semiconductor nanostructure are replaced by cations of different metals with preservation of the shape and the anionic framework of the nanocrystals. Utilizing this cation exchange method, we synthesized two new tetrapods for the first time: Cu2-xSe/Cu2-xS and PbSe/PbS, both prepared from CdSe/CdS tetrapods as `templates'. We also fabricated near-infrared (NIR) photodetectors with a very simple architecture comprising a PbSe/PbS tetrapod layer between two Au electrodes on a glass substrate. When illuminated by a NIR laser, these devices are capable of achieving a responsivity of 11.9 A W-1 without the use of ligand-exchange processes, thermal annealing or hybrid device architecture. Transient absorption spectroscopy was carried out on these PbSe/PbS tetrapods, the results of which suggest that the branched morphology contributes in part to device performance. Investigation of the charge dynamics of the PbSe/PbS tetrapods revealed an extremely long-lived exciton recombination lifetime of ~17 ms, which can result in enhanced photoconductive gain. Overall, these heterostructured tetrapods showcase simultaneously the importance of nanoparticle shape, band structure, and surface chemistry in the attainment of NIR photodetection.In this work we explore the preparation of complex-shaped semiconductor nanostructures composed of different materials via a cationic exchange process in which the cations of the original semiconductor nanostructure are replaced by cations of different metals with preservation of the shape and the anionic framework of the nanocrystals. Utilizing this cation exchange method, we synthesized two new tetrapods for the first time: Cu2-xSe/Cu2-xS and PbSe/PbS, both prepared from CdSe/CdS tetrapods as `templates'. We also fabricated near-infrared (NIR) photodetectors

  12. An anionic zeolite-like metal-organic framework (AZMOF) with a Moravia network for organic dye absorption through cation-exchange.

    PubMed

    Shen, Yu; Fan, Cong-Cong; Wei, Yu-Zhen; Du, Jie; Zhu, Hai-Bin; Zhao, Yue

    2016-07-01

    An anionic zeolite-like metal-organic framework (AZMOF) with a twisted partially augmented the net, known as the "Moravia" net, [(CH3)2NH2]6[Sr13(O)3()8(OH)2(H2O)16]·xS (, where S represents non-coordinated solvent molecules, and is the abbreviation of benzo-(1,2;3,4;5,6)-tris-(thiophene-2'-carboxylic acid)), has been solvothermally synthesized and characterized, which possesses an anionic framework and nano-sized sodalite cage. Through cation-exchange, is capable of uptaking large organic cationic dyes including Rhodamine B (RB), Basic Red 2 (BR2), Crystal Violet (CV) and Methylene Blue (MB), amongst which the adsorption capability for RB (up to 545 mg g(-1)), and BR2 (up to 675 mg g(-1)) is the highest for reported absorbants to date. PMID:27301344

  13. Synthesis of Capsule-like Porous Hollow Nanonickel Cobalt Sulfides via Cation Exchange Based on the Kirkendall Effect for High-Performance Supercapacitors.

    PubMed

    Tang, Yongfu; Chen, Shunji; Mu, Shichun; Chen, Teng; Qiao, Yuqing; Yu, Shengxue; Gao, Faming

    2016-04-20

    To construct a suitable three-dimensional structure for ionic transport on the surface of the active materials for a supercapacitor, porous hollow nickel cobalt sulfides are successfully synthesized via a facile and efficient cation-exchange reaction in a hydrothermal process involving the Kirkendall effect with γ-MnS nanorods as a sacrificial template. The formation mechanism of the hollow nickel cobalt sulfides is carefully illustrated via the tuning reaction time and reaction temperature during the cation-exchange process. Due to the ingenious porous hollow structure that offers a high surface area for electrochemical reaction and suitable paths for ionic transport, porous hollow nickel cobalt sulfide electrodes exhibit high electrochemical performance. The Ni1.77Co1.23S4 electrode delivers a high specific capacity of 224.5 mAh g(-1) at a current density of 0.25 A g(-1) and a high capacity retention of 87.0% at 10 A g(-1). An all-solid-state asymmetric supercapacitor, assembled with a Ni1.77Co1.23S4 electrode as the positive electrode and a homemade activated carbon electrode as the negative electrode (denoted as NCS//HMC), exhibits a high energy density of 42.7 Wh kg(-1) at a power density of 190.8 W kg(-1) and even 29.4 Wh kg(-1) at 3.6 kW kg(-1). The fully charged as-prepared asymmetric supercapacitor can light up a light emitting diode (LED) indicator for more than 1 h, indicating promising practical applications of the hollow nickel cobalt sulfides and the NCS//HMC asymmetric supercapacitor. PMID:27031254

  14. Effect of bore fluid composition on microstructure and performance of a microporous hollow fibre membrane as a cation-exchange substrate.

    PubMed

    Lazar, R A; Mandal, I; Slater, N K H

    2015-05-15

    Micro-capillary film (MCF) membranes are effective platforms for bioseparations and viable alternatives to established packed bed and membrane substrates at the analytical and preparative chromatography scales. Single hollow fibre (HF) MCF membranes with varied microstructures were produced in order to evaluate the effect of the bore fluid composition used during hollow fibre extrusion on their structure and performance as cation-exchange adsorbers. Hollow fibres were fabricated from ethylene-vinyl alcohol (EVOH) copolymer through solution extrusion followed by nonsolvent induced phase separation (NIPS) using bore fluids of differing composition (100wt.% N-methyl-2-pyrrolidone (NMP), 100wt.% glycerol, 100wt.% water). All HFs displayed highly microporous and mesoporous microstructures, with distinct regions of pore size <1μm, 5-15μm and up to 50μm in diameter, depending upon proximity to the bore fluid. Scanning electron microscopy (SEM) revealed skins of pore size <1μm at the inner surface of HFs produced with water and glycerol, while NMP bore fluid resulted in a skinless inner HF surface. The HFs were modified for chromatography by functionalising the polymer surface hydroxyl groups with sulphonic acid (SP) groups to produce cation-exchange adsorbers. The maximum binding capacities of the HFs were determined by frontal analysis using lysozyme solutions (0.05-100mgml(-1)) for a flow rate of 1.0mlmin(-1). The NMP-HF-SP module displayed the largest maximum lysozyme binding capacity of all the fibres produced (40.3mg lysozyme/ml adsorbent volume), a nearly 2-fold increase over the glycerol and 10-fold increase over the water variants at the same sample flow rate. The importance of NMP as a bore fluid to hollow fibre membrane performance as a result of inner surface porosity was established with a view to applying this parameter for the optimisation of multi-capillary MCF performance in future studies. PMID:25840664

  15. On the real performance of cation exchange resins in wastewater treatment under conditions of cation competition: the case of heavy metal pollution.

    PubMed

    Prelot, Benedicte; Ayed, Imen; Marchandeau, Franck; Zajac, Jerzy

    2014-01-01

    Sorption performance of cation-exchange resins Amberlite® IRN77 and Amberlite™ IRN9652 toward Cs(I) and Sr(II) has been tested in single-component aqueous solutions and simulated waste effluents containing other monovalent (Effluent 1) or divalent (Effluent 2) metal cations, as well as nitrate, borate, or carbonate anions. The individual sorption isotherms of each main component were measured by the solution depletion method. The differential molar enthalpy changes accompanying the ion-exchange between Cs+ or Sr2+ ions and protons at the resin surface from single-component nitrate solutions were measured by isothermal titration calorimetry and they showed a higher specificity of the two resins toward cesium. Compared to the retention limits of both resins under such idealized conditions, an important depression in the maximum adsorption capacity toward each main component was observed in multication systems. The overall effect of ion exchange process appeared to be an unpredictable outcome of the individual sorption capacities of the two resins toward various cations as a function of the cation charge, size, and concentration. The cesium retention capacity of the resins was diminished to about 25% of the "ideal" value in Effluent 1 and 50% in Effluent 2; a further decrease to about 15% was observed upon concomitant strontium addition. The uptake of strontium by the resins was found to be less sensitive to the addition of other metal components: the greatest decrease in the amount adsorbed was 60% of the ideal value in the two effluents for Amberlite® IRN77 and 75% for Amberlite™ IRN9652. It was therefore demonstrated that any performance tests carried out under idealized conditions should be exploited with much caution to predict the real performance of cation exchange resins under conditions of cation competition. PMID:24728575

  16. LA-ICP-MS of rare earth elements concentrated in cation-exchange resin particles for origin attribution of uranium ore concentrate.

    PubMed

    Asai, Shiho; Limbeck, Andreas

    2015-04-01

    Rare earth elements (REE) concentrated on cation-exchange resin particles were measured with laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to obtain chondrite-normalized REE plots. The sensitivity of REE increased in ascending order of the atomic number, according to the sensitivity trend in pneumatic nebulization ICP-MS (PN-ICP-MS). The signal intensities of REE were nearly proportional to the concentrations of REE in the immersion solution used for particle-preparation. Minimum measurable concentration calculated from the net signals of REE was approximately 1 ng/g corresponding to 0.1 ng in the particle-preparation solution. In LA analysis, formation of oxide and hydroxide of the light REE and Ba which causes spectral interferences in the heavy REE measurement was effectively attenuated due to the solvent-free measurement capability, compared to conventional PN-ICP-MS. To evaluate the applicability of the proposed method, the REE-adsorbed particles prepared by immersing them in a U-bearing solution (commercially available U standard solution) were measured with LA-ICP-MS. Aside from the LA analysis, each concentration of REE in the same U standard solution was determined with conventional PN-ICP-MS after separating REE by cation-exchange chromatography. The concentrations of REE were ranging from 0.04 (Pr) to 1.08 (Dy) μg/g-U. The chondrite-normalized plot obtained through LA-ICP-MS analysis of the U standard sample exhibited close agreement with that obtained through the PN-ICP-MS of the REE-separated solution within the uncertainties. PMID:25640124

  17. Development of Online pH Gradient-Eluted Strong Cation Exchange Nanoelectrospray-Tandem Mass Spectrometry for Proteomic Analysis Facilitating Basic and Histidine-Containing Peptides Identification.

    PubMed

    Xu, Jingjing; Gao, Jing; Yu, Chengli; He, Han; Yang, Yiming; Figeys, Daniel; Zhou, Hu

    2016-01-01

    A novel one-dimensional online pH gradient-eluted strong cation exchange-nanoelectrospray ionization-tandem mass spectrometry (SCX-nano-ESI-MS/MS) method was developed for protein identification and tested with a mixture of six standard proteins, total lysate of HuH7 and N2a cells, as well as membrane fraction of N2a cells. This method utilized an online nanoflow SCX column in a nano-LC system coupled with a nanoelectrospray high-resolution mass spectrometer. Protein digests were separated on a nanoflow SCX column with a pH gradient and directly introduced into a mass spectrometer through nanoelectrospray ionization. More than five thousand unique peptides were identified in each 90 min LC-MS/MS run using 500 nanogram of protein digest either from total cell lysate or from membrane fraction. The unique peptide overlap between online strong cation exchange nano-ESI-MS/MS (SCXLC-MS/MS) and reverse phase nano-ESI-MS/MS (RPLC-MS/MS) is only ≤30%, which indicated these two methods were complementary to each other. The correlation coefficient of retention time and theoretical isoelectric point (pI) of identified peptides in SCXLC-MS/MS was higher than 0.4, which showed that peptides elution in SCXLC-MS/MS was dependent on their charge states. Furthermore, SCXLC-MS/MS showed identification capability for a higher proportion of basic peptides compared to the RPLC-MS/MS method, especially for histidine-containing peptides. Our SCXLC-MS/MS method is an excellent alternative method to the RPLC-MS/MS method for analysis of standard proteins, total cell and membrane proteomes. PMID:26646553

  18. Use of Cation Exchange Resins for Production of U{sub 3}O{sub 8} Suitable for the Al-U{sub 3}O{sub 8} Powder Metallurgy Process

    SciTech Connect

    Mosley, W.C.

    2001-09-17

    This report describes the production of U{sub 3}O{sub 8} powders from three types of cation exchange resins: Dowex 50W, a strong acid, sulfonate resin; AG MP-50, a macroporous form of sulfonate resin; and Bio-Rex 70, a weak acid, carboxylic resin.

  19. The polymerization and electrochemical characterization of polypyrrole and polypyrrole/poly(ethylene oxide)pyrrole copolymers

    NASA Astrophysics Data System (ADS)

    Huntoon, Trey William Stevens

    1998-11-01

    The work contained within this document discusses the polymerization and subsequent characterization of Polypyrrole based electrodes for lithium batteries. Polypyrrole and Polypyrrole/polyethyloxy copolymers were compared and contrasted in an attempt to show the superior kinetics of the copolymer electrode. It was found that the diffusion of dopant ions across the electrode and electrolyte interface was increased by on order of magnitude in the copolymer sample. It was also found that the reversibility of the Polypyrrole electrode was greater than that of the copolymer electrode. While the diffusion coefficient of the copolymer electrode was altered to be comparable to that of the transition metal oxide cathodes in production today, the capacity of the copolymer material is still too low to be considered as an alternative cathode material in the lithium battery industry.

  20. Electrorheological characteristics of polypyrrole-based suspensions

    NASA Astrophysics Data System (ADS)

    Huang, Weijiu

    2005-12-01

    In this paper, electrorheological (ER) suspensions containing polypyrrole particles and castor oil were prepared. The rheological and conductive properties of these polypyrrole-based suspensions and their influencing factors, such as electric field strength, particle concentration, temperature and shear rate, were investigated as well. The experimental results show that with increasing electric field strength, particle concentration and shear rate, the shear stress of the suspension is enhanced; while with an increasing temperature, the shear stress of a suspension decreases. The conductive properties of the suspension was found to increase with an increase of electric field strength, particle concentration and temperature, but decrease with shear rate.

  1. Chitosan-Polypyrrole Fiber for Strain Sensor.

    PubMed

    Lee, Songjun; Yi, Byung-Ju; Chun, Kyoung-Yong; Lee, Jaeah; Kim, Youn Tae; Cha, Eun-Jong; Kim, Seon Jeong

    2015-03-01

    A chitosan/polypyrrole composited fiber as bio-compatible materials for artificial muscles is investigated. The chitosan/polypyrrole fiber (CPF) is fabricated by in-situ chemical polymerization of pyrrole monomer solution using FeCl3 as an oxidant. The electrical resistivity of the fiber is changed according to the strain variation applied to the both ends of the specimen. The sensor built by using the CPF has a higher gauge factor (4) compared to conventional metal strain gauges (~2) indicating a suitable material for delicate force control in sensing work. PMID:26413701

  2. Synthesis and characterization of aluminium–alumina micro- and nano-composites by spark plasma sintering

    SciTech Connect

    Dash, K. Chaira, D.; Ray, B.C.

    2013-07-15

    Graphical abstract: The evolution of microstructure by varying the particle size of reinforcement in the matrix employing spark plasma sintering has been demonstrated here in Al–Al{sub 2}O{sub 3} system. An emphasis has been laid on varying the reinforcement particle size and evaluating the microstructural morphologies and their implications on mechanical performance of the composites. Nanocomposites of 0.5, 1, 3, 5, 7 volume % alumina (average size < 50 nm) reinforced in aluminium matrix were fabricated by powder metallurgy route using spark plasma sintering technique technique at a temperature of 773 K and pressure of 50 MPa. Another set of specimens having composition 1, 5, 20 vol.% of alumina (average size ∼ 10 μm) had been fabricated to compare the physical as well as mechanical attributes of the microcomposite as well as the nanocomposites. These micro- and nano-composites have been characterized using X-ray diffraction, scanning electron microscopy and transmission electron microscopy followed by density, microhardness and nanoindentation measurements. The alumina nanoparticles revealed an interface showing appreciable physical intimacy with the aluminium matrix compared to that of the alumina microparticles. The interfacial integrity in case of nanocomposites is better than in the microcomposite which has been studied using microscopic techniques. Spark plasma sintering imparts enhanced densification as well as matrix-reinforcement proximity which has been corroborated with the experimental results. - Highlights: • The Al–Al{sub 2}O{sub 3} micro- and nano-composites fabricated by spark plasma sintering. • Better matrix-reinforcement integrity in nanocomposites than microcomposites. • Spark plasma sintering method results in higher density and hardness values. • High density and hardness values of nanocomposites than microcomposites. • High dislocation density in spark plasma sintered Al–Al{sub 2}O{sub 3} composites. - Abstract: In the

  3. Metal chalcogenide nanoparticle gel networks: Their formation mechanism and application for novel material generation and heavy metal water remediation via cation exchange reactions

    NASA Astrophysics Data System (ADS)

    Palhares, Leticia F.

    The dissertation research is focused on (1) uncovering the mechanism of metal chalcogenide nanoparticle gel formation; (2) extending the cation exchange reaction protocol to zinc sulfide gel networks, with the goal of accessing new aerogel chemistries and understanding the factors that drive the process; and (3) conducting a quantitative analysis of the ability of ZnS aerogels to remove heavy metal ions from aqueous solutions. The mechanism of metal chalcogenide nanoparticle gel formation was investigated using Raman spectroscopy and X-ray Photoelectron Spectroscopy to probe the chemical changes that occur during the gelation process. These techniques suggest that the bonding between the particles in the CdSe nanoparticle gels is due to the oxidation of surface selenide species, forming covalent Se--Se bonds. Treating the gel networks with a suitable reducing agent, such as a thiol, breaks the covalent bond and disperses the gel network. The addition of sodium borohydride, a "pure" reducing agent, also breaks down the gel network, strengthening the hypothesis that the reducing character of the thiols, not their ligation ability, is responsible for the gel network breakdown. UV-Vis spectroscopy, Transmission Electron Microscopy and Powder X-ray Diffraction were used to analyze the particles after successive gelation-dispersion cycles. The primary particle size decreases after repeated oxidation-reduction cycles, due to nanoparticle surface etching. This trend is observed for CdSe and CdS gel networks, allowing for the proposition that the oxidative-reductive mechanism responsible for the formation-dispersion of the gels is general, applying to other metal chalcogenide nanocrystals as well. The cation exchange reaction previously demonstrated for CdSe gels was extended to ZnS gel networks. The exchange occurs under mild reaction conditions (room temperature, methanol solvent) with exchanging ions of different size, charge and mobility (Ag+, Pb2+, Cd2+ , Cu2+). The

  4. High pressure synthesis of novel, zeolite based nano-composite materials

    NASA Astrophysics Data System (ADS)

    Santoro, Mario

    2013-06-01

    Meso/micro-porous solids such as zeolites are complex materials exhibiting an impressive range of applications, including molecular sieve, gas storage, catalysis, electronics and photonics. We used these materials, particularly non catalytic zeolites in an entirely different fashion. In fact, we performed high pressure (0.5-30 GPa) chemical reactions of simple molecules on a sub-nanometer scale in the channels of a pure SiO2 zeolite, silicalite to obtain unique nano-composite materials with drastically modified physical and chemical properties. Our material investigations are based on a combination of X-ray diffraction and optical spectroscopy techniques in the diamond anvil cell. I will first briefly show how silicalite can be easily filled by simple molecules such as Ar, CO2 and C2H4 among others from the fluid phase at high pressures, and how this efficient filling removes the well known pressure induced amorphization of the silica framework (Haines et al., JACS 2010). I will then present on a silicon carbonate crystalline phase synthesized by reacting silicalite and molecular CO2 that fills the nano-pores, at 18-26 GPa and 600-980 K; after the synthesis the compound is temperature quenched and it results to be slightly metastable at room conditions (Santoro et al., PNAS 2011). On the other hand, a stable at room condition spectacular crystalline nano-composite is obtained by photo-polymerizing ethylene at 0.5-1.5 GPa under UV (351-364 nm) irradiation in the channels of silicalite (Santoro et al., Nat. Commun, in press 2013). For this composite we obtained a structure with single polyethylene chains adapting very well to the confining channels, which results in significant increases in bulk modulus and density, and the thermal expansion coefficient changes sign from negative to positive with respect to the original silicalite host. Mechanical properties may thus be tuned by varying the amount of polymerized ethylene. We then think our findings could allow the

  5. Evolution with time of hydrophobicity and microrelief of a cation-exchange membrane surface and its impact on overlimiting mass transfer.

    PubMed

    Pismenskaya, Natalia D; Nikonenko, Victor V; Melnik, Nadezhda A; Shevtsova, Kseniya A; Belova, Elena I; Pourcelly, Gérald; Cot, Didier; Dammak, Lasâad; Larchet, Christian

    2012-02-23

    Surface properties were measured together with electrochemical characteristics of a CMX (Neosepta, Tokuyama Corp.) cation-exchange membrane. Relative hydrophobicity was controlled by the contact angle; XPS and SEM were used for characterizing chemical composition and microrelief of the surface, respectively. Voltammetry, chronopotentiometry, and mass transfer rate measurements were made as well. A "fresh" membrane and samples after 10, 25, 100, and 150 h of operation in an electrodialysis cell at an overlimiting current equal to 3 theoretical limiting currents, in a 0.02 M NaCl solution, were characterized. Some electrochemical properties were also measured for a Neosepta cation-exchange membrane, aged 2 years, in an industrial food process. It was found that the hydrophobicity of the CMX membrane has increased after the first 10 h of operation; more and more cavities of the dimension of the order of 1 μm have appeared with time testifying electrochemical erosion of the surface. The limiting current density (i(lim)) and the overlimiting transfer rate through the CMX membrane increased with time of its operation under overlimiting current. In the case of new CMX, i(lim) was very close to the theoretical value i(lim)(theor) calculated by the Lévêque equation. After 10 h of operation, i(lim) increased by 5%, and after 25, 100, and 150 h, the increase was by 30%, 70%, and 100%, respectively. Similarly, the mass transfer rate was found to increase up to 5 times (when desalting 0.005 M NaCl under 3 V) in comparison with the theoretical value. The ensemble of data was explained by the hypothesis that the passage of intensive current produces erosion of the ion-exchange polymer forming a continuous phase in CMX. This erosion results in exposure at the surface of the other constituent of CMX: small (about 100 nm) particles of relatively hydrophobic polyvinylchloride. Increasing surface hydrophobicity facilitates the slip of electroconvective vortexes along the surface

  6. Design of a fixed-bed ion-exchange process for the treatment of rinse waters generated in the galvanization process using Laminaria hyperborea as natural cation exchanger.

    PubMed

    Mazur, Luciana P; Pozdniakova, Tatiana A; Mayer, Diego A; Boaventura, Rui A R; Vilar, Vítor J P

    2016-03-01

    In this study, the removal of zinc from galvanization wastewaters was performed in a fixed bed column packed with brown macro-algae Laminaria hyperborea, acting as a natural cation exchanger (resin). The rinse wastewater presents a zinc concentration between 9 and 22 mg/L, a high concentration of light metals (mainly Na and Ca), a high conductivity (0.5-1.5 mS/cm) and a low organic content (DOC = 7-15 mg C/L). The zinc speciation diagram showed that approximately 80% of zinc is in the form of Zn(2+) and ≅20% as ZnSO4, considering the effluent matrix. From all operational conditions tested for zinc uptake (17 < bed height<27 cm, 4.5 < flow rate<18.2 BV/h, 0.8 < particle equivalent diameter<2.0 mm), the highest useful capacity (7.1 mg Zn/g algae) was obtained for D/dp = 31, L/D = 11, 9.1 BV/h, τ = 6.4 min, corresponding to a service capacity of 124 BV (endpoint of 2 mg Zn/L). Elution was faster and near to 100% effective using 10 BV of HCl (1 M, 3.0%, 363 g HCl/L of resin), for flow rates higher than 4.5 BV/h. Calcium chloride solution (0.1 M) was selected as the best regenerant, allowing the reuse of the natural resin for more than 3 saturation/elution/regeneration cycles. The best operation conditions were scaled-up and tested in a pre-pilot plant. The scale-up design of the cation exchange process was proposed for the treatment of 2.4 m(3)/day of galvanization wastewater, resulting in an estimated reactants cost of 2.44 €/m(3). PMID:26766159

  7. Molecular Dynamics Study on the Particle Dispersion Mechanism of Polyamide-imide/Silica Nano-composite Materials

    NASA Astrophysics Data System (ADS)

    Kikuchi, Hideyuki; Iwasaki, Tomio; Hanawa, Hidehito; Honda, Yuki

    We studied the particle dispersion mechanism of polyamide-imide/silica nano-composite material by using molecular-dynamics simulation technique based on Newtonian dynamics and quantum mechanics. In simulations, adhesive fracture energies at the interfaces between silica and solvents were calculated, and Brownian motions of silica particles were simulated to clarify dispersion properties. The simulation results showed that the colloidal state of silica was maintained by covering the silica surface with a new low hygroscopicity solvent and that the chemical structure of polymer contributed to the dispersion of silica. It is found that the results obtained from molecular dynamics agree well with those obtained by experiments, and that molecular-dynamics simulation technique will become very useful for the development of nano-composite materials in the future.

  8. High-Pressure Synthesis of Metal-Ceramic Nano-Composites

    NASA Technical Reports Server (NTRS)

    Gierlotka, S.; Palosz, B.; Ekimov, E.; Grzanka, E.; Stelmakh, S.; Lojkowski, W.; Bismayer, U.; Palosz, W.; Rose, M. Franklin (Technical Monitor)

    2001-01-01

    The major problems in fabrication of nano-crystal line materials form nano-powders are: (1), coarsening of the initial nano-size grains, (2), insufficient densification (high concentration of pores), and, (3), conversion of diamond into graphite (for diamond-based ceramics). We have developed a novel technique of the synthesis of nano-composite materials applying very high (up to about 10 GPa) pressures. In this technique, one component is pre-compacted and placed next to another having a lower melting point temperature. The whole sample is pressed and the temperature raised above the melting point of the second component, what results in the melt getting pressed into the (nano-size) pores of the compact. Upon subsequent crystallization the melt forms the second nanophase. The process is fast, on the order of seconds, and the temperatures are relatively low what prevents, or at least significantly reduces coarsening of the starting nanophase grains. Also, conversion of diamond into graphite can be prevented. The technique allows for control of the final product properties through a proper selection of (1) the initial compact density and grain size, (2) chemical composition of the source, and (3) the temperature and pressure of the process. The application of the technique to the synthesis of SiC and diamond with Si, Ge, and different metals. Results of the in-situ investigation of the synthesis process by synchrotron X-ray diffraction technique will be presented.

  9. Apatite-forming ability of a zirconia/alumina nano-composite induced by chemical treatment.

    PubMed

    Uchida, Masaki; Kim, Hyun-Min; Kokubo, Tadashi; Nawa, Masahiro; Asano, Taiyo; Tanaka, Kenji; Nakamura, Takashi

    2002-05-01

    Induction of an apatite-forming ability on a nano-composite of a ceria-stabilized tetragonal zirconia polycrystals (Ce-TZP) and alumina (Al2O3) polycrystals via chemical treatment with aqueous solutions of H3PO4, H2SO4, HCl, or NaOH has been investigated. The Ce-TZP/Al2O3 composite is attractive as a load-bearing bone substitute because of its mechanical properties. The chemical treatments produced Zr-OH surface functional groups, which are known to be effective for apatite nucleation in a body environment. The composite, after chemical treatment, was shown to form a bonelike apatite layer when immersed in a simulated body fluid containing ion concentrations nearly equal to those in human blood plasma. This implies that it may form apatite in the living body and bond to living bone through the apatite layer. This type of bioactive Ce-TZP/Al2O3 composite is therefore expected to be useful as a bone substitute, even under load-bearing conditions. PMID:11857434

  10. Synthesis and characterization of liposomes nano-composite-particles with hydrophobic magnetite as a MRI probe

    NASA Astrophysics Data System (ADS)

    Han, Limin; Zhou, Xingping

    2016-07-01

    Nano-magnetic liposomes (MLs) consist of liposomes and magnetic nanoparticles (MNPs). Due to the active surfaces of liposomes, various functional groups can be attached for ligand-specific targeting. Here, we describe synthesis of magnetic nano-composite liposomes (HMLs) by a thin film dispersing method, based on hydrophobic magnetite (Fe3O4) nanoparticles. The results showed that the particle diameter of the HMLs containing Fe3O4sbnd OA NPs at a final Fe loading of 11.02 g/mol phosphatidylcholine (POPC) mainly in a sandwich-structure was 125.3 ± 12.9 nm determined by transmission electron microscopy (TEM) and dynamic light scattering (DLS). While the initial Fe concentration in the solution varied from 0.25 to 3.0 mg/mL, an effective Fe3O4 NPs loading was achieved, with encapsulation efficiency (EE%) from 91.0% to 71.0%. Subsequently, the HMLs were confirmed to be quite cytocompatible and hemocompatible in the applied concentration range by MTT and hemolysis assays. We also found that HMLs had more advantages than those liposomes with hydrophilic Fe3O4 NPs by comparing their EE% and r2 relaxivity. Finally, it was concluded that the analyzed Fe concentration in HMLs was sufficient to produce a pronouncedly weak signal for MRI in vitro to enhance the contrast between tumors and normal tissues.

  11. Preparation and characterization of PVP-PVA-ZnO blend polymer nano composite films

    NASA Astrophysics Data System (ADS)

    Divya, S.; Saipriya, G.; Hemalatha, J.

    2016-05-01

    Flexible self-standing films of PVP-PVA blend composites are prepared by using ZnO as a nano filler at different concentrations. The structural, compositional, morphological and optical studies made with the help of X-ray diffraction (XRD), Fourier Transform Infra-Red spectroscopy (FTIR), Scanning electron microscope (SEM), Atomic Force Microscopy (AFM), Ultraviolet-visible spectroscopy (UV-vis) and Photoluminescence (PL) spectra are presented in this paper. The results of XRD indicate that ZnO nanoparticles are formed with hexagonal phase in the polymeric matrix. SEM images show the dispersion of ZnO nano filler in the polymer matrix. UV-vis spectra reveal that the absorption peak is centered around 235nm and 370nm for the nano composite films. The blue shift is observed with decrease in the concentration of the nano filler. PL spectra shows the excitation wavelength is given at 320nm.The emission peaks were observed at 383 nm ascribing to the electronic transitions between valence band and conduction band and the peak at 430 nm.

  12. Synthesis, characterization and band gap energy of poly(ɛ-caprolactone)/Sr-MSA nano-composite

    NASA Astrophysics Data System (ADS)

    Kannammal, L.; Palanikumar, S.; Meenarathi, B.; Yelilarasi, A.; Anbarasan, R.

    2014-04-01

    A mercaptosuccinic acid (MSA) decorated Sr nano-particle (NP) was prepared and characterized by using various analytical techniques and was used as a chemical initiator for the ring opening polymerization (ROP) of ɛ-caprolactone (CL). The ROP of CL was carried out at various experimental conditions under N2 atmosphere with mild stirring. The initiating efficiency of MSA-decorated Sr NP was tested in terms of Fourier transform infrared-relative intensity, melting temperature (Tm), degradation temperature (Td) and molecular weight (Mw) of poly(ɛ-caprolactone) (PCL), differential scanning calorimetry, UV-visible spectroscopy, field emission scanning electron microscopy, thermogravimetric analysis and gel permeation chromatography analytical techniques. The nuclear magnetic resonance spectrum confirms the chemical structure of PCL. While increasing the [M/I] ratio, the Mw of PCL was linearly increased. The band gap energy of Sr was determined from the UV-visible spectrum. The reflectance study proves the hydrophobic nature of the Sr-hybrid and its nano-composite formation with PCL.

  13. Molecular organic crystalline matrix for hybrid organic-inorganic (nano) composite materials

    NASA Astrophysics Data System (ADS)

    Stanculescu, A.; Tugulea, L.; Alexandru, H. V.; Stanculescu, F.; Socol, M.

    2005-02-01

    Metal-doped benzil crystals have been grown by thermal gradient solidification in a vertical transparent growth configuration to investigate the effect of metallic guest on the ordered organic host. We have identified the conditions for growing homogeneous, optically good crystals of benzil doped with sodium and silver, limiting the effect of supercooling, low thermal conductivity and anisotropy of the growth speed (temperature gradient at the liquid-solid interface: 10-25 °C, moving speed of the growth interface 2.0 mm/h). The nature and concentration of the dopant are parameters affecting, through the growth process, the crystalline perfection and the optical properties of the organic matrix. Bulk optical characterisation, by spectrophotometrical methods, has offered details on some intrinsic properties of the system metal particles/benzil crystalline matrix. Analytical processing of the experimental data emphasised that benzil is a wide optical band gap organic semiconductor Eg=2.65 eV. We also have investigated the effect of sodium and silver on the properties of benzil crystal as potential transparent semiconductor matrix for (nano)composite metal/molecular organic material. With the increase of sodium concentration from c=1 to 6 wt%, a small narrowing of the band gap has been remarked. The same behaviour has been found for benzil doped with silver (c=2 wt%) compared to pure benzil.

  14. A Micro/Nano Composite for Combination Treatment of Melanoma Lung Metastasis.

    PubMed

    Mi, Yu; Mu, Chaofeng; Wolfram, Joy; Deng, Zaian; Hu, Tony Ye; Liu, Xuewu; Blanco, Elvin; Shen, Haifa; Ferrari, Mauro

    2016-04-01

    The successful treatment of malignant disease generally requires the use of multiple therapeutic agents that are coordinated in a spatiotemporal manner to enable synergy. Here, a porous silicon-based micro/nano composite (MNC) that is capable of simultaneously delivering chemotherapeutic agents and small interfering RNA (siRNA) to the lungs following intravenous injection is designed. The pores of the silicon microparticles are loaded with B-Raf proto-oncogene serine/threonine kinase (BRAF) siRNA-containing liposomes, while the surface is conjugated with docetaxel-encapsulated polymeric nanoparticles. The synergistic antitumor effect of the MNC is demonstrated in vitro in melanoma cells and in vivo using a mouse model for melanoma lung metastasis. The MNC displays superior therapeutic efficacy and increased accumulation in metastatic melanoma lesions in the lungs in comparison to combination therapy with liposomes and polymers. The results indicate that the MNC can be used as an effective delivery vehicle for simultaneous enrichment of multiple therapeutic agents in the lungs. PMID:26890862

  15. Magnetite/graphene oxide nano-composite for enhancement of hydrogen production from gelatinaceous wastewater.

    PubMed

    Mostafa, Alsayed; El-Dissouky, Ali; Fawzy, Amal; Farghaly, Ahmed; Peu, Pascal; Dabert, Patrick; Le Roux, Sophie; Tawfik, Ahmed

    2016-09-01

    The effect of substrate to inoculum (So/Xo) ratio and supplementation of magnetite/graphene oxide (MGO) nano-composite material on hydrogen production from gelatinaceous wastewater via dark fermentation process was investigated. Results demonstrated that optimum So/Xo ratio of 1.0gCOD/gVSS achieved maximal hydrogen yield (HY) of 79.2±11.9mL H2/gCOD removed. Supplementation of anaerobes with 100mg/L MGO promoted HY up to 112.4±10.5mL H2/gCOD removed. Moreover, the degradation efficiency of carbohydrates, proteins and lipids was improved to 80.8±7.6, 34.4±2.3 and 31.4±2.2%, respectively. Acetate (HAc) and butyrate (HBu) concentrations increased from 102±6.8 to 125.3±6.3 and from 31.1±1.5 to 48.8±3.5mg/gVSS, respectively. However, propionate (HPr) concentration dropped from 35.9±2.7 to 15±1.3mg/gVSS. Hydrogenase enzyme activity increased 9-folds and the anaerobes elongated from ca. 1.8-2.9 to ca. 2.5-5.1μm with MGO addition. Moreover, Proteobacteria, Firmicutes, Clostridia and Bacilli were detected with the batches supplemented with MGO. PMID:27268437

  16. Isolation of carboxyl-termini and blocked amino-termini of viral proteins by high-performance cation-exchange chromatography.

    PubMed

    Gorman, J J; Shiell, B J

    1993-08-27

    The strong cation-exchanger, PolySulfoethyl Aspartamide, has been assessed as a medium for isolation of carboxyl-terminal and blocked amino-terminal peptides from tryptic digests of small quantities of viral proteins. Peptides with a single positive charge, the blocked amino-terminal peptides of ovalbumin and the Newcastle disease virus (NDV) matrix protein and carboxyl-terminal peptides of ovalbumin and the NDV nucleocapsid protein, eluted in early ion-exchange fractions and were readily isolated in homogeneous form by subsequent reversed-phase HPLC. Some early ion-exchange fractions also contained singly charged peptides derived by "chymotryptic-like" cleavage, whilst other peptides eluted in these fractions due to their highly acidic character. Terminal sequences with additional basic residues were isolated from later eluting ion-exchange fractions. Peptides with this property included the blocked amino-terminus of the NDV nucleocapsid protein and a portion of the carboxyl-terminus of the NDV matrix protein. Hitherto undescribed polymorphism in the amino-terminal region of ovalbumin was revealed in this study. Truncated peptides from the carboxyl-terminus of the NDV matrix protein were also detected. The presence of these peptides could be a reflection of carboxyl-terminal processing of the matrix protein. The strategy described herein should be of general utility for selective microisolation of carboxyl-terminal peptides and blocked amino-terminal peptides from tryptic digests of proteins. PMID:8408428

  17. Modeling and robust pooling design of a preparative cation-exchange chromatography step for purification of monoclonal antibody monomer from aggregates.

    PubMed

    Borg, Niklas; Brodsky, Yan; Moscariello, John; Vunnum, Suresh; Vedantham, Ganesh; Westerberg, Karin; Nilsson, Bernt

    2014-09-12

    This study has implemented and calibrated a model that describes the separation of the monomer of monoclonal antibodies from the dimer and larger oligomers on preparative-scale using cation-exchange chromatography. A general rate model with temperature dependent diffusion was coupled to a pH- and temperature-dependent steric mass action model. The model was shown to predict the retention of the monomer, dimer, and oligomer at low loadings for different pH levels and temperatures. Additionally, the model was shown to adequately predict the elution behavior of the monomer and soluble aggregates at high loadings within the same ranges with some limitations. The model was not able to accurately describe the shape of the product break-through curves or the slight levels of co-elution of the dimer and oligomer with the monomer at higher pH. The model was used to predict how 12 process variations impact the separation. The model is used to establish an elution end collection criterion such that the step can robustly provide the target purity of monomers. PMID:25085821

  18. Multistep mineral fouling growth on a cation-exchange membrane ruled by gradual sieving effects of magnesium and carbonate ions and its delay by pulsed modes of electrodialysis.

    PubMed

    Cifuentes-Araya, Nicolás; Pourcelly, Gérald; Bazinet, Laurent

    2012-04-15

    The aim of this study was to reveal the mechanisms ruling a fouling growth on both sides of a CMX-SB cation-exchange membrane (CEM), run after run during three consecutive electrodialysis (ED) treatments. A model solution containing a high magnesium/calcium ratio (2/5) was demineralized under two different pulsed electric field (PEF) on-duty ratios and dc current. The results showed a series of mechanisms ruling a multilayer mineral fouling growth and its delay by PEFs. The nature of the fouling layer, during a first run, depended on the diluate pH-value evolutions and the ion migration rates through the membrane. A subsequent multilayer fouling growth during consecutive treatments was ruled by the already formed mineral layers, where gradual sieving effects inverted the migration rates and led to a multistep crystal growth. Calcium carbonate grew on the diluate side of CEM, starting from its amorphous phase to then crystallize in a coexisting presence of aragonite and calcite. Amorphous magnesium hydroxide appeared on CEM apparently through fouling dehydration ruled by the mineral layers themselves and by overlimiting current regimes. A delayed fouling growth was observed for PEF ratio 0.3. A long pause lapse during pulse modes was demonstrated as an important parameter for fouling mitigation. PMID:22326231

  19. Mixed-mode anion-cation exchange/hydrophilic interaction liquid chromatography-electrospray mass spectrometry as an alternative to reversed phase for small molecule drug discovery

    PubMed

    Strege; Stevenson; Lawrence

    2000-10-01

    Within pharmaceutical drug discovery, significant needs currently exist for the analysis and purification of structurally diverse samples prior to or immediately following high-throughput screening. These processes are required to facilitate rapid and accurate biological profiling, structural determination, and resupply of new drug candidates. Reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with electrospray ionization mass spectrometry (ESI-MS) for both analytical and preparative applications has become the small molecule separation/detection tool of choice for meeting many of these needs. However, the separation selectivity provided by RP-HPLC has been limited to the hydrophobicity-based resolution of relatively nonpolar sample components, and for high-throughput drug discovery applications, no sufficient alternative procedures have been identified. In this investigation, a mixed-mode anion-cation exchange/hydrophilic interaction chromatography (ACE-HILIC) method has been developed to provide both direct compatibility with ESI-MS and evaporative light-scattering detection (ELSD) and separation selectivity highly orthogonal to RP-HPLC. The technique employed silica-based small-pore weak ion exchange resins eluted with a combined aqueous and pH gradient. A diverse set of dipeptide probes was employed for the elucidation of the relative contributions of three retention mechanisms. ACE-HILIC-ESI-MS-ELSD should prove useful for the analysis and purification of compounds from both biological (e.g., natural products) and synthetic (e.g., combinatorial chemistry) sources of molecular diversity. PMID:11028621

  20. Quantification of Site-Specific Cation Exchange in Metal-Organic Frameworks Using Multi-Wavelength Anomalous X-ray Dispersion

    SciTech Connect

    Brozek, Carl K.; Cozzolino, Anthony F.; Teat, Simon J.; Chen, Yu-Sheng; Dinc,; #259; Mircea,

    2013-09-23

    We employed multiwavelength anomalous X-ray dispersion to determine the relative cation occupation at two crystallographically distinct metal sites in Fe2+-, Cu2+-, and Zn2+-exchanged versions of the microporous metal–organic framework (MOF) known as MnMnBTT (BTT = 1,3,5-benzenetristetrazolate). By exploiting the dispersive differences between Mn, Fe, Cu, and Zn, the extent and location of cation exchange were determined from single crystal X-ray diffraction data sets collected near the K edges of Mn2+ and of the substituting metal, and at a wavelength remote from either edge as a reference. Comparing the anomalous dispersion between these measurements indicated that the extent of Mn2+ replacement depends on the identity of the substituting metal. We contrasted two unique methods to analyze this data with a conventional approach and evaluated their limitations with emphasis on the general application of this method to other heterometallic MOFs, where site-specific metal identification is fundamental to tuning catalytic and physical properties.

  1. Rapid method of separating Am(VI) from transplutonium and rare-earth elements on a cation exchanger in phosphoric acid

    SciTech Connect

    Tikhomirova, G.S.; Guseva, L.I.

    1988-07-01

    Measurements have been made on cation-exchanger sorption of americium, other actinoids, and certain rare-earth elements from 0.1-2.0 M H/sub 3/PO/sub 4/ when the elements have been oxidized with ammonium persulfate alone or mixed with silver phosphate. There are considerable differences in behavior between the americium and the other elements on account of its being oxidized to a higher valency state. Measurements have been made on the effects of acid and oxidant concentrations and of the oxidation and elution conditions on the americium yield when the exchanger is treated with H/sub 3/PO/sub 4/. Optimum oxidation conditions have been chosen, and a rapid method has been devised for separating americium(VI) from other transplutonium elements and REE on Dowex 50 /times/ 8, where the eluent is 0.1-1.0 M H/sub 3/PO/sub 4/ plus 0.05 M (NH/sub 4/)/sub 2/S/sub 2/O/sub 8/.

  2. [Effects of biochar amendment on cropland soil bulk density, cation exchange capacity, and particulate organic matter content in the North China Plain].

    PubMed

    Chen, Hong-Xia; Du, Zhang-Liu; Guo, Wei; Zhang, Qing-Zhong

    2011-11-01

    A 3-year field experiment with randomized block design was conducted to study the effects of biochar amendment on the soil bulk density, cation exchange capacity (CEC), and particulate organic matter C (POM-C) and N (POM-N) contents in a high-yielding cropland in the North China Plain. Four treatments were installed, i.e., chemical NPK (CK), chemical NPK plus 2250 kg x hm(-2) of biochar (C1), chemical NPK plus 4500 kg x hm(-2) of biochar (C2), and 750 kg x hm(-2) of biochar-based slow release fertilizer (CN). Comparing with CK, treatments C1 and C2 significantly decreased the bulk density of 0-7.5 cm soil layer by 4.5% and 6.0%, respectively, and the treatments with biochar amendment increased the CEC in 0-15 cm soil layer, with an increment of 24.5% in treatment C2. Biochar amendment also increased the C (POM-C) and N (POM-N) contents in 0-7.5 cm soil layer, e.g., the POM-C and N contents in treatment C1 and C2 were 250% and 85%, and 260% and 120% higher than those of the CK, respectively. After three years of biochar amendment, the soil had obvious improvement in its physical and chemical properties, and played more active roles in soil carbon sequestration and greenhouse gases emission reduction. PMID:22303671

  3. A comparative study on textural characterization: cation-exchange and sorption properties of crystalline alpha-zirconium(IV), tin(IV), and titanium(IV) phosphates.

    PubMed

    Parida, K M; Sahu, B B; Das, D P

    2004-02-15

    Tetravalent metal phosphates (M=Zr, Ti, and Sn) were prepared and characterized by XRD, surface properties, and TG-DTA. The cation exchange and sorption behavior of these metal phosphates toward transition metal ions such as Cu(2+), Co(2+), and Ni(2+) have been studied comparatively as a function of temperature and concentration. The adsorption process was found to increases with increase in temperature and concentration. The selectivity order for alpha-titanium and alpha-tin phosphates is Cu(2+)>Co(2+)>Ni(2+), whereas for alpha-zirconium phosphate it is Cu(2+)>Ni(2+)>Co(2+). The ion exchange capacity of alpha-titanium phosphate is greater than those of other phosphates, which is explained on the basis of the surface behavior, disorderness of the system, degree of hydrolysis of incoming guest adsorbate metal ions, and structural steric hindrance of the exchangers during adsorption and sorption. The distribution coefficient, Gibbs free energy, enthalpy, and entropy values indicate that the ion-exchange processes are spontaneous. PMID:14697711

  4. Selective and Accurate Determination Method of Propofol in Human Plasma by Mixed-Mode Cation Exchange Cartridge and GC-MS.

    PubMed

    Pyo, Jae Sung

    2016-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for the determination of propofol in human plasma has been developed and validated. Propofol was extracted from human plasma by using mixed-mode cation exchange/reversed-phase (MCX) cartridges. As propofol easily volatilizes during concentration, 100% methanol was injected directly into GC-MS to elute propofol. Despite avoiding concentration process of the eluted solution, lower limit of quantization (LLOQ) of propofol was 25 ng/mL. The validated method exhibited good linearity (R (2) = 0.9989) with accuracy and precision -5.8%~11.7% and 3.7%~11.6%, respectively. The other validation parameters, recovery and matrix effect, ranged from 96.6% to 99.4% and 95.3% to 101.4%, respectively. Propofol standard was quantified to evaluate possible loss due to the concentration processes, nitrogen gas and centrifugal vacuum. These two concentration processes resulted in notable decrease in the quantity of propofol, signifying avoiding any concentration processes during propofol quantification. Also, to confirm suitability of the developed method, authentic human plasma samples were analyzed. The selective assay method using MCX cartridge and GC-MS facilitated quantification of propofol in plasma sample accurately by preventing any losses due to the concentration processes. PMID:27597928

  5. Quantitative determination of 22 primary aromatic amines by cation-exchange solid-phase extraction and liquid chromatography-mass spectrometry.

    PubMed

    Aznar, Margarita; Canellas, Elena; Nerín, Cristina

    2009-07-01

    Primary aromatic amines (PAAs) have been broadly studied due to their high toxicity. In this work a method for the analysis of 22 PAAs in aqueous simulants has been developed. The method is based on a solid-phase extraction step using cation-exchange cartridges and the subsequent analysis of the extracts by ultra-high-performance liquid chromatography with mass spectrometric detection. The recoveries obtained for all the amines analyzed ranged between 81 and 109%, linear range was between 0.03 and 75 microg L(-1), with the RSD values between 4.5 and 13.4% and an average value of 7.5% and limits of detection at microg L(-1) level. The method has been applied to two real samples obtained from migration experiments of polyurethane based laminates to simulant B (water with 3% (w/v) acetic acid) which represents the worst case for the migration of aromatic amines. The main amines found in both samples were methylenedianiline isomers, obtained from the corresponding residual diisocyanates used during polyurethane adhesive polymerization. The total amine concentration found was 26 and 6.3 microg of aniline equivalents per kg of food simulant. PMID:19464690

  6. Selective sorption of lead, cadmium and zinc ions by a polymeric cation exchanger containing nano-Zr(HPO3S)2.

    PubMed

    Zhang, Qingrui; Pan, Bingcai; Pan, Bingjun; Zhang, Weiming; Jia, Kun; Zhang, Quanxing

    2008-06-01

    A novel polymeric hybrid sorbent, namely ZrPS-001, was fabricated for enhanced sorption of heavy metal ions by impregnating Zr(HPO3S)2 (i.e., ZrPS) nanoparticles within a porous polymeric cation exchanger D-001. The immobilized negatively charged groups bound to the polymeric matrix D-001 would result in preconcentration and permeation enhancement of target metal ions prior to sequestration, and ZrPS nanoparticles are expected to sequester heavy metals selectively through an ion-exchange process. Highly effective sequestration of lead, cadmium, and zinc ions from aqueous solution can be achieved by ZrPS-001 even in the presence of competing calcium ion at concentration several orders of magnitude greater than the target species. The exhausted ZrPS-001 beads are amenable to regeneration with 6 M HCI solution for repeated use without any significant capacity loss. Fixed-bed column treatment of simulated waters containing heavy metals at high or trace levels was also performed. The content of heavy metals in treated effluent approached or met the WHO drinking water standard. PMID:18589978

  7. Review of the thermal stability and cation exchange properties of the zeolite minerals clinoptilolite, mordenite, and analcime; applications to radioactive waste isolation in silicic tuff

    SciTech Connect

    Smyth, J.R.; Caporuscio, F.A.

    1981-06-01

    Silicic tuffs of the southern Great Basin and basalts of the Columbia River Plateau are under investigation as potential host rocks for high- and intermediate-level radioactive wastes. Nonwelded and partially welded tuffs may contain major amounts (> 50%) of the zeolite minerals clinoptilolite, mordenite, and analcime. Densely welded tuffs and some basalt flows may contain clinoptilolite as fracture filling that limits the permeability of these rocks. The cation exchange properties of these zeolite minerals allow them to pose a formidable natural barrier to the migration of cationic species of various radionuclides in aqueous solutions. However, these minerals are unstable at elevated temperatures and at low water-vapor pressures and may break down either by reversible dehydration or by irreversible mineralogical reactions. All the breakdown reactions occurring at increased temperature involve a net volume reduction and evolution of fluids. Thus, they may provide a pathway (shrinkage fractures) and a driving force (fluid pressure) for release of radionuclides to the biosphere. These reactions may be avoided by keeping zeolite-bearing horizons saturated with water and below about 85{sup 0}C. This may restrict allowable gross thermal loadings in waste repositories in volcanic rocks.

  8. Double-peak elution profile of a monoclonal antibody in cation exchange chromatography is caused by histidine-protonation-based charge variants.

    PubMed

    Luo, Haibin; Cao, Mingyan; Newell, Kelcy; Afdahl, Christopher; Wang, Jihong; Wang, William K; Li, Yuling

    2015-12-11

    We have systemically investigated unusual elution behaviors of an IgG4 (mAb A) in cation exchange chromatography (CEX). This mAb A exhibited two elution peaks under certain conditions when being purified by several strong CEX columns. When either of the two peaks was isolated and re-injected on the same column, the similar pattern was observed again during elution. The protein distribution between the two peaks could be altered by NaCl concentration in the feed, or NaCl concentration in wash buffer, or elution pH, suggesting two pH-associated strong-and-weak binding configurations. The protein distributions under different pH values showed good correlation with protonated/un-protonated fractions of a histidine residue. These results suggest that the double-peak elution profile associates with histidine-protonation-based charge variants. By conducting pepsin digestion, amino-acid specific chemical modifications, peptide mapping, and measuring the effects of elution residence time, a histidine in the variable fragment (Fab) was identified to be the root cause. Besides double-peak pattern, mAb A can also exhibit peak-shouldering or single elution peak on different CEX resins, reflecting different resins' resolving capability on protonated/un-protonated forms. This work characterizes a novel cause for unusual elution behaviors in CEX and also provides alternative avenues of purification development for mAbs with similar behaviors. PMID:26596869

  9. Selective and Accurate Determination Method of Propofol in Human Plasma by Mixed-Mode Cation Exchange Cartridge and GC-MS

    PubMed Central

    2016-01-01

    A gas chromatography-mass spectrometry (GC-MS) method for the determination of propofol in human plasma has been developed and validated. Propofol was extracted from human plasma by using mixed-mode cation exchange/reversed-phase (MCX) cartridges. As propofol easily volatilizes during concentration, 100% methanol was injected directly into GC-MS to elute propofol. Despite avoiding concentration process of the eluted solution, lower limit of quantization (LLOQ) of propofol was 25 ng/mL. The validated method exhibited good linearity (R2 = 0.9989) with accuracy and precision −5.8%~11.7% and 3.7%~11.6%, respectively. The other validation parameters, recovery and matrix effect, ranged from 96.6% to 99.4% and 95.3% to 101.4%, respectively. Propofol standard was quantified to evaluate possible loss due to the concentration processes, nitrogen gas and centrifugal vacuum. These two concentration processes resulted in notable decrease in the quantity of propofol, signifying avoiding any concentration processes during propofol quantification. Also, to confirm suitability of the developed method, authentic human plasma samples were analyzed. The selective assay method using MCX cartridge and GC-MS facilitated quantification of propofol in plasma sample accurately by preventing any losses due to the concentration processes. PMID:27597928

  10. Ultra-High-Efficiency Strong Cation Exchange LC/RPLC/MS/MS for High Dynamic Range Characterization of the Human Plasma Proteome

    SciTech Connect

    Shen, Yufeng; Jacobs, Jon M.; Camp, David G.; Fang, Ruihua; Moore, Ronald J.; Smith, Richard D.; Xiao, Wenzhong; Davis, Ronald W.; Tompkins, Ronald G.

    2004-02-15

    In this study, we report a comprehensive approach for ultrahigh-efficiency separations by liquid chromatography (LC)/tandem mass spectrometry (MS/MS) for broad protein characterization of human plasma. The power of this approach is demonstrated by the confident identification of 1062 human plasma proteins based upon identification of 2992 tryptic peptides using highly conservative SEQUEST search criteria from a non-depleted human plasma sample. The approach provides a dynamic range of {approx}9 orders of magnitude in protein abundance using conventional ion trap MS/MS, which enabled identification of pg/mL concentration human plasma proteins (e.g. cytokines) co-existing with mg/mL-level human serum albumin. This dynamic range was obtained by combining high-efficiency reversed-phase (RP) LC coupled with efficient pre-fractionation strong cation exchange (SCX) LC to achieve ultrahigh-efficiency separations. A single-dimension, high-efficiency RPLC provided a protein identification dynamic range of 4 orders of magnitude in protein content and identified 433 human plasma proteins; while the ultrahigh-efficiency SCXLC/RPLC (i.e. 15 fractions from SCXLC), with the assistance of the SCXLC-sample component concentration (up to 102 fold), extended the protein identification dynamic range to {approx}9 orders of magnitude in protein content, identifying 822 human plasma proteins; combination of single- and two-dimension LC/MS/MS led to identification of 1062 human plasma proteins.

  11. A facile route to violet- to orange-emitting CdxZn1-xSe alloy nanocrystals via cation exchange reaction

    NASA Astrophysics Data System (ADS)

    Zhong, Xinhua; Feng, Yaoyu; Zhang, Yuliang; Gu, Zhenyu; Zou, Lei

    2007-09-01

    The most advanced CdSe-based binary semiconductor system does not work well for emission in the short wavelength spectral region from 420 to 500 nm, which is of special interest for the preparation of nanocrystal-based blue LEDs and white light generation. CdxZn1-xSe alloy nanocrystals are proven to be an attractive alternative as their emission color can be tuned from the UV spectral region (ZnSe) to the red region (CdSe) by changing the composition of the Zn/Cd ratio in the alloy. Herein we report a facile and 'green' alloying approach for the preparation of highly luminescent CdxZn1-xSe nanocrystals via cation exchange reaction of the pre-prepared ZnSe nanocrystals with Cd2+ at intermediate temperatures. Through this new synthetic strategy, high-quality alloy QDs with different desired emission wavelengths or colors (ranging from 370 to 600 nm) can be made reproducibly and precisely by varying the predetermined amounts of the reaction precursors.

  12. Conducting molecular composites of polypyrrole with electroactive polymeric dopantions

    SciTech Connect

    Cameron, D.A.; Reynolds, J.R.

    1996-10-01

    Polypyrrole is one of the most widely used and studied electroactive polymers due to its good conductivity and stability in air. A variety of low molecular weight and polymeric ions have been used as charge compensating dopants in conductive polypyrrole in its oxidized state. In this work we report the electro-polymerization of polypyrrole films incorporating electroactive N-substituted polyaniline polyelectrolytes as dopant ions.

  13. Synthesis and characterization of Zn-B-Si-O nano-composites and their doped BaTiO{sub 3} ceramics

    SciTech Connect

    Niu, Ruiyuan; Cui, Bin; Du, Fengtao; Chang, Zhuguo; Tang, Zongxun

    2010-10-15

    We synthesized Zn-B-Si-O (ZBSO) nano-composites via sol-gel process, and then used them to dope BaTiO{sub 3} ceramics. The ZBSO nano-composites and their ceramics were characterized by means of thermogravimetric, Fourier-transform infrared, and X-ray diffraction methods, and using scanning and transmission electron microscopy. We also characterized the dielectric properties of the ceramics. The results indicated that the ZBSO nano-composites were nanometer-scale powders with an amorphous structure. The particle size of the powders increased with increasing pH value, but initially decreased and then increased with increasing calcining temperature. At pH about 2 and with calcining at 400 {sup o}C, the nano-composites attained minimum particle size (about 30 nm). The sintering temperature of the BaTiO{sub 3} ceramics could be reduced to 1100 {sup o}C by adding 5 wt% of the ZBSO nano-composites. Uniform, fine-grained BaTiO{sub 3} ceramics with a high permittivity ({epsilon}{sub r} = 2946 and {epsilon}{sub max} = 5072) were obtained by adding nano-composites; these properties were superior to the ZBSO glass doped BaTiO{sub 3} ceramics.

  14. Metal | polypyrrole battery with the air regenerated positive electrode

    NASA Astrophysics Data System (ADS)

    Grgur, Branimir N.

    2014-12-01

    Recharge characteristics of the battery based on the electrochemically synthesized polypyrrole cathode and aluminum, zinc, or magnesium anode in 2 M NH4Cl are investigated. It is shown that polypyrrole electrode can be regenerated by the reoxidation with the dissolved oxygen from the air. Using the polypyrrole synthesized on high surface graphite-felt electrode under modest discharge conditions, stable discharge voltage of 1.1 V is obtained. Such behavior is explained by the complex interaction of polypyrrole and hydrogen peroxide produced by the oxygen reduction reaction. The electrochemical characteristics are compared with the zinc-manganese dioxide and zinc-air systems.

  15. The nano-composite nature of vanadium oxide thin films for use in infrared microbolometers

    NASA Astrophysics Data System (ADS)

    Gauntt, Bryan Douglas

    2011-12-01

    The current generation of portable, un-cooled infrared imaging devices utilizes thin-film materials with large thermal coefficients of resistivity. Incoming photons are absorbed by the material, converted into heat, and result in a decrease in the resistivity of the thermal sensing layer. Vanadium oxide thin films are used in the majority of these devices as they typically have very large thermal coefficients of resistivity with low noise characteristics. In the work reported here, reactive pulsed DC sputtering was used to grow a systematic series of vanadium oxide thin films with resistivity ranging from 1 x 10-3 to 6.8 x 104 Ohm cm and TCR varying from 0 to 4% K-1. Throughout the parameter space studied, a transition from amorphous to nano-crystalline growth was observed. Films in the range of interest for a microbolometer, i.e. 1 x 10-3 to 10 Ohm cm, contain the face-centered cubic (FCC) VO x (0.8 < x < 1.3) phase. Films with larger resistivity were found to be amorphous. Stoichiometry measurements via Rutherford backscattering spectroscopy place many of the nano-crystalline films outside of the FCC VO x phase field according to the bulk phase diagram. Electron diffraction in the transmission electron microscope confirmed the presence of a secondary oxygen-rich amorphous vanadium oxide phase. The oxygen-rich amorphous phase explains the discrepancy between the observed oxygen content, which is outside of the FCC VOx phase field, and the presence of FCC VOx, which is limited to a maximum oxygen content of x = 1.3. The resulting microstructure can be described as a nano-composite material composed of a low resistivity crystalline phase embedded in a high resistivity amorphous matrix. A mechanism has been proposed wherein the nano-composite structure of the films results from film growth in alternating oxygen deficient and oxygen rich regions in the chamber. While in the oxygen deficient region the nano-crystalline phase grows preferentially, and while in the

  16. The diametral tensile strength and hydrostability of polymer-ceramic nano-composite (pcnc) material prototypes

    NASA Astrophysics Data System (ADS)

    Yepez, Johanna

    Statement of the problem: There is a weak connection between the filler and the resin matrix of dental composites caused primarily by hydrolysis of silane coupling agent, therefore, jeopardizing the mechanical properties of the dental restorations. Purpose: The purpose of this study was to compare the diametral tensile strength (DTS) of a nano-mechanically bonded polymer ceramic nano composite (pcnc) versus the chemically bonding prototype polymer ceramic nano composite (pcnc) fabricated by using hydrolytically stable interphase. Materials and Methods: Composites were made with 60wt % filler, 38% triethyleneglycol dimethacrylate (TEDGMA), 1% camphorquinone (CQ) and 1% 2-(dimethylamino) ethyl methacrylate (DMAEMA). Tests for DTS were performed using a universal testing machine. The disk-shaped specimens were loaded in compression between two supporting plates at a crosshead speed of 0.5 mm/min until fracture. The samples, measuring 3 mm in height and 6 mm in diameter, were produced in a round stainless steel (SS) mold. A total of 144 samples were created. Groups of 48 samples were made for each of three different fillers. Specimens were soaked in artificial saliva at 37° for four time periods, dry(t=0), 1 day, 7 days, 28 days). At the end of each soaking time DTS tests were performed. Results: There where statistically significant differences in the DTS between the filler groups and the soaking times (p=<0.001) as well as for the pairwise comparison between the different filler group values and between the different soaking times as an individual treatment. Overall, longer soaking times resulted in lower mean DTS values. The DTS of the PCNC for filler #1 decreased to 82.4% of the original value after 1 day of soaking, 67.2% after 7 days and 27.2 % after 28 days. For filler #2 decreased to 54.8% of the original value after 1 day of soaking, 62.3% after 7 days and 61.2% after 28 days. For filler #3 decreased to 71.2% of the original value, 67.3% after 7 days and 51

  17. Synthesis, characterization and magnetic behavior of Co/MCM-41 nano-composites

    SciTech Connect

    Cuello, N.; Elías, V.; Crivello, M.; Oliva, M.; Eimer, G.

    2013-09-15

    Synthesis, structure and magnetic properties of Co/MCM-41 as magnetic nano-composites have been investigated. Mesoporous materials with different degrees of metal loading were prepared by wet impregnation and characterized by ICP, XRD, N{sub 2} adsorption, UV–vis DRS, TPR and EPMA-EDS. Cobalt oxide clusters and Co{sub 3}O{sub 4} nano-particles could be confined inside the mesopores of MCM-41, being this fact favored by the Co loading increasing. In addition, larger crystals of Co{sub 3}O{sub 4} detectable by XRD also grow on the surface when the Co loading is enhanced. The magnetic characterization was performed in a SQUID magnetometer using a maximum magnetic applied field µ{sub 0}Ha=1 T. While the samples with the higher Co loadings showed a behavior typically paramagnetic, a superparamagnetic contribution is more notorious for lower loadings, suggesting high Co species dispersion. - Graphical abstract: Room temperature hysteresis loops as a function of the Co content. Display Omitted - Highlights: • Co species as isolated Co{sup 2+}, oxide clusters and Co{sub 3}O{sub 4} nano-particles were detected. • For higher Co loads were detected, by XRD, Co{sub 3}O{sub 4} particles on the external surface. • The confining of Co species inside the mesopores was achieved by increasing Co load. • Paramagnetism from oxide clusters/nano-particles becomes dominant for higher Co loads. • Superparamagnetism can be assigned to Co species of small size and finely dispersed.

  18. Influence of mouth rinses on the surface hardness of dental resin nano-composite

    PubMed Central

    Khan, Aftab Ahmed; Siddiqui, Adel Zia; Mohsin, Syed Fareed; Al-Kheraif, Abdulaziz A.

    2015-01-01

    Objective: The aim of this research was to assess the effect of mouth rinses with and without alcohol on the hardness of dental nano-filled composite. Methods: The micro-hardness of fifty circular disk shaped specimens of 7 mm x 2 mm were measured after 14 days. Specimens were immersed into alcohol containing (Listerine and Colgate Perioguard) and alcohol-free (Prodent and Sensodyne Oral antiseptic) mouth rinse solutions. Artificial saliva served as the control. Vickers Micro-hardness was measured with a 30gram load for 30 seconds dwell time by using a diamond indenter. Significant differences were represented by p<0.05, whereas highly significant difference represented by p<0.01. The level of significance (p) was calculated with the help of repeated measure ANOVA. For multiple comparisons, Tukey’s multiple comparison test was used. Results: Statistical analysis revealed highly significant difference between specimens immersed in artificial saliva (control) and Listerine (p<0.01). Whereas significant difference were observed between control and Colgate Periogard (p<0.05). However, no significant difference was observed on comparing Prodent and Sensodyne Oral antiseptic mouth rinses with control group(p>0.05). Control specimens depicted highest value of micro-hardness(60.5746 ± 3.2703) compared to the lowest value seen in specimens immersed in Listerine solvent(54.4687 ± 1.0937). Conclusion: Alcohol containing mouth rinsing solutions have more deleterious effect on hardness of nano composites as compared to alcohol-free mouth rinses. PMID:26870121

  19. Organic polymer-metal nano-composites for opto-electronic sensing of chemicals in agriculture

    NASA Astrophysics Data System (ADS)

    Sarkisov, Sergey S.; Czarick, Michael; Fairchild, Brian D.; Liang, Yi; Kukhtareva, Tatiana; Curley, Michael J.

    2013-03-01

    Recent research findings led the team to conclude that a long lasting and inexpensive colorimetric sensor for monitoring ammonia emission from manure in confined animal feeding operations could eventually become feasible. The sensor uses robust method of opto-electronic spectroscopic measurement of the reversible change of the color of a sensitive nano-composite reagent film in response to ammonia. The film is made of a metal (gold, platinum, or palladium) nano-colloid in a polymer matrix with an ammonia-sensitive indicator dye additive. The response of the indicator dye (increase of the optical absorption in the region 550 to 650 nm) is enhanced by the nano-particles (~10 nm in size) in two ways: (a) concentration of the optical field near the nano-particle due to the plasmon resonance; and (b) catalytic acceleration of the chemical reaction of deprotonization of the indicator dye in the presence of ammonia and water vapor. This enhancement helps to make a miniature and rugged sensing element without compromising its sensitivity of less than 1 ppm for the range 0 to 100 ppm. The sensor underwent field tests in commercial broiler farms in Georgia, Alabama, and Arkansas and was compared against a commercial photoacoustic gas analyzer. The sensor output correlated well with the data from the photoacoustic analyzer (correlation coefficient not less than 0.9 and the linear regression slope after calibration close to 1.0) for several weeks of continuous operation. The sources of errors were analyzed and the conclusions on the necessary improvements and the potential use of the proposed device were made.

  20. Use of potassium-form cation-exchange resin as a conductimetric enhancer in ion-exclusion chromatography of aliphatic carboxylic acids.

    PubMed

    Iwata, Tomotaka; Mori, Masanobu; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2009-09-15

    In this study, a cation-exchange resin (CEX) of the K(+)-form, i.e., an enhancer resin, is used as a postcolumn conductimetric enhancer in the ion-exclusion chromatography of aliphatic carboxylic acids. The enhancer resin is filled in the switching valve of an ion chromatograph; this valve is usually used as a suppressor valve in ion-exchange chromatography. An aliphatic carboxylic acid (e.g., CH(3)COOH) separated by a weakly acidic CEX column of the H(+)-form converts into that of the K(+)-form (e.g., CH(3)COOK) by passing through the enhancer resin. In contrast, the background conductivity decreases because a strong acid (e.g., HNO(3)) with a higher conductimetric response in an eluent converts into a salt (e.g., KNO(3)) with a lower conductimetric response. Since the pH of the eluent containing the resin enhancer increases from 3.27 to 5.85, the enhancer accelerates the dissociations of analyte acids. Consequently, peak heights and peak areas of aliphatic carboxylic acids (e.g., acetic acid, propionic acid, butyric acid, and valeric acid) with the enhancer resin are 6.3-8.0 times higher and 7.2-9.2 times larger, respectively, than those without the enhancer resin. Calibrations of peak areas for injected analytes are linear in the concentration range of 0.01-1.0mM. The detection limits (signal-to-noise ratio=3) range from 0.10 microM to 0.39 microM in this system, as opposed to those in the range of 0.24-7.1 microM in the separation column alone. The developed system is successfully applied to the determination of aliphatic carboxylic acids in a chicken droppings sample. PMID:19615503

  1. Physical characterization of the state of motion of the phenalenyl spin probe in cation-exchanged faujasite zeolite supercages with pulsed EPR

    NASA Astrophysics Data System (ADS)

    Doetschman, D. C.; Dwyer, D. W.; Fox, J. D.; Frederick, C. K.; Scull, S.; Thomas, G. D.; Utterback, S. G.; Wei, J.

    1994-08-01

    The molecular motion of the phenalenyl (PNL) spin probe in the supercages of cation-exchanged X and Y zeolites (faujasites) has been physically characterized by pulsed and continuous wave (CW) electron paramagnetic resonance (EPR). Both X and Y zeolites, whose cation sites were exchanged with the alkali metal ions, Li +, Na +, K +, Rb + and Cs + were examined. There is a good correspondence between the temperature dependences of the PNL electron spin phase memory time and the CW EPR spectra. Both display evidence of a thermal activation from a stationary, non-rotating molecular state to a low-temperature state of in-plane rotation (Das et al., Chem Phys. 143 (1990) 253). The rate of in-plane rotation is an activated process, with E* | / R=1289 |+- 35 K and 1462 ± 47 K in NaX and KX zeolites, respectively. The rotation appears to be about an axis along which the half-filled, non-bonding π orbital interacts with the exchanged cation in the supercage. Both CW and pulsed EPR also show a higher temperature activation from the in-plane rotating state to an effectively isoptropic state of rotation of PNL in which the PNL-cation bond is thought to be broken, with E* ⊥ / R=2050 ± 110 K, 1956 ± 46K, 1335 ± 97 K in LiX, NaX and KX zeolites, respectively. The strength of the PNL-cation bonding decreases with increasing cation atomic number as indicated by E* ⊥ and the peripheral repulsion (crowding) of PNL increases with cation size as indicated E* |. There are qualitative indications that the binding of PNL to the cations in the Y zeolite is stronger than in the X zeolite.

  2. 2-Acrylamido-2-methyl-1-propanesulfonic Acid Grafted Poly(vinylidene fluoride-co-hexafluoropropylene)-Based Acid-/Oxidative-Resistant Cation Exchange for Membrane Electrolysis.

    PubMed

    Pandey, Ravi P; Das, Arindam K; Shahi, Vinod K

    2015-12-30

    For developing acid-/oxidative-resistant aliphatic-polymer-based cation-exchange membrane (CEM), macromolecular modification of poly(vinylidene fluoride-co-hexafluoropropylene) (PVDF-co-HFP) was carried out by controlled chemical grafting of 2-acrylamido-2-methyl-1-propanesulfonic acid (AMPS). To introduce the unsaturation suitable for chemical grafting, dehydrofluorination of commercially available PVDF-co-HFP was achieved under alkaline medium. Sulfonated copolymer (SCP) was prepared by the free radical copolymerization of dehydofluorinated PVDF-co-HFP (DHPVDF-co-HFP) and AMPS in the presence of free radical initiator. Prepared SCP-based CEMs were analyzed for their morphological characteristics, ion-exchange capacity (IEC), water uptake, conductivity, and stabilities (mechanical, chemical, and thermal) in comparison with state-of-art Nafion117 membrane. High bound water content avoids the membrane dehydration, and most optimal (SCP-1.33) membrane exhibited about ∼2.5-fold high bound water content in comparison with that of Nafion117 membrane. Bunsen reaction of iodine-sulfur (I-S) was successfully performed by direct-contact-mode membrane electrolysis in a two-compartment electrolytic cell using different SCP membranes. High current efficiency (83-99%) confirmed absence of any side reaction and 328.05 kJ mol-H2(-1) energy was required for to produce 1 mol of H2 by electrolytic cell with SCP-1.33 membrane. In spite of low conductivity for reported SCP membrane in comparison with that of Nafion117 membrane, SCP-1.33 membrane was assessed as suitable candidate for electrolysis because of its low-cost nature and excellent stabilities in highly acidic environment may be due to partial fluorinated segments in the membrane structure. PMID:26642107

  3. A novel approach to measure elemental concentrations in cation exchange resins using XRF-scanning technique, and its potential in water pollution studies

    NASA Astrophysics Data System (ADS)

    Huang, Jyh-Jaan; Lin, Sheng-Chi; Löwemark, Ludvig; Liou, Ya-Hsuan; Chang, Queenie; Chang, Tsun-Kuo; Wei, Kuo-Yen; Croudace, Ian W.

    2016-04-01

    X-ray fluorescence (XRF) core-scanning is a fast, and convenient technique to assess elemental variations for a wide variety of research topics. However, the XRF scanning counts are often considered a semi-quantitative measurement due to possible absorption or scattering caused by down core variability in physical properties. To overcome this problem and extend the applications of XRF-scanning to water pollution studies, we propose to use cation exchange resin (IR-120) as an "elemental carrier", and to analyze the resins using the Itrax-XRF core scanner. The use of resin minimizes the matrix effects during the measurements, and can be employed in the field in great numbers due to its low price. Therefore, the fast, and non-destructive XRF-scanning technique can provide a quick and economical method to analyze environmental pollution via absorption in the resin. Five standard resin samples were scanned by the Itrax-XRF core scanner at different exposure times (1 s, 5 s, 15 s, 30 s, 100 s) to allow the comparisons of scanning counts with the absolute concentrations. The regression lines and correlation coefficients of elements that are generally used in pollution studies (Ca, Ti, Cr, Ni, Cu, Zn, and Pb) were examined for the different exposure times. The result shows that within the test range (from few ppm to thousands ppm), the correlation coefficients are all higher than 0.97, even at the shortest exposure time (1 s). Therefore, we propose to use this method in the field to monitor for example sewage disposal events. The low price of resin, and fast, multi elements and precise XRF-scanning technique provide a viable, cost- and time-effective approach that allows large sample numbers to be processed. In this way, the properties and sources of wastewater pollution can be traced for the purpose of environmental monitoring and environmental forensics.

  4. High-purity isolation of anthocyanins mixtures from fruits and vegetables--a novel solid-phase extraction method using mixed mode cation-exchange chromatography.

    PubMed

    He, Jian; Giusti, M Monica

    2011-11-01

    Research on biological activity of anthocyanins requires the availability of high purity materials. However, current methods to isolate anthocyanins or anthocyanin mixtures are tedious and expensive or insufficient for complete isolation. We applied a novel cation-exchange/reversed-phase combination solid-phase extraction (SPE) technique, and optimized the use of water/organic buffer mobile phases to selectively separate anthocyanins. Crude extracts of various representative anthocyanin sources were purified with this technique and compared to 3 commonly used SPE techniques: C(18), HLB, and LH-20. Purified anthocyanin fractions were analyzed with high performance liquid chromatography (HPLC) coupled to photodiode array (PDA) and mass spectrometry (MS) detectors and by Fourier transform infrared (FT-IR) spectroscopy. The UV-visible chromatograms quantitatively demonstrated that our novel technique achieved significantly higher (P<0.05) anthocyanin purity than the C(18) cartridge, the next best method, for 11 of the 12 anthocyanin sources tested. Among them, eight were purified to greater than 99% purity (based on UV-visible chromatograms). The new method efficiently removed non-anthocyanin phenolics. MS and FT-IR results semi-quantitatively confirmed extensive reduction of impurities. Due to strong ionic interaction, our sorbent capacity was superior to others, resulting in the highest throughput and least use of organic solvents. This new methodology for isolation of anthocyanin mixtures drastically increased purity and efficiency while maintaining excellent recovery rate and low cost. The availability of high purity anthocyanin mixtures will facilitate anthocyanin studies and promote the application of anthocyanins in the food and nutraceutical industries. PMID:21968344

  5. Integrated strong cation-exchange hybrid monolith coupled with capillary zone electrophoresis and simultaneous dynamic pH junction for large-volume proteomic analysis by mass spectrometry.

    PubMed

    Zhang, Zhenbin; Sun, Liangliang; Zhu, Guijie; Yan, Xiaojing; Dovichi, Norman J

    2015-06-01

    A sulfonate-silica hybrid strong cation-exchange (SCX) monolith was synthesized at the proximal end of a capillary zone electrophoresis column and used for on-line solid-phase extraction (SPE) sample preconcentration. Sample was prepared in an acidic buffer and deposited onto the SCX-SPE monolith and eluted using a basic buffer. Electrophoresis was performed in an acidic buffer. This combination of buffers results in formation of a dynamic pH junction, which allows use of relatively large elution buffer volume while maintaining peak efficiency and resolution. All experiments were performed with a 50 µm ID capillary, a 1cm long SCX-SPE monolith, a 60cm long separation capillary, and a electrokinetically pumped nanospray interface. The volume of the capillary is 1.1 µL. By loading 21 µL of a 1×10(-7) M angiotensin II solution, an enrichment factor of 3000 compared to standard electrokinetic injection was achieved on this platform while retaining efficient electrophoretic performance (N=44,000 plates). The loading capacity of the sulfonate SCX hybrid monolith was determined to be ~15 pmol by frontal analysis with 10(-5) M angiotensin II. The system was also applied to the analysis of a 10(-4) mg/mL bovine serum albumin tryptic digest; the protein coverage was 12% and 11 peptides were identified. Finally, by loading 5.5 µL of a 10(-3) mg/mL E. coli digest, 109 proteins and 271 peptides were identified in a 20 min separation; the median separation efficiency generated by these peptides was 25,000 theoretical plates. PMID:25863379

  6. LC-MS/MS analysis of pramipexole in mouse plasma and tissues: elimination of lipid matrix effects using weak cation exchange mode based solid-phase extraction.

    PubMed

    Guo, Weilin; Li, Gao; Yang, Yanxia; Yang, Conglian; Si, Luqin; Huang, Jiangeng

    2015-04-15

    Intranasal delivery is emerging as a promising alternative for oral or intravenous administration of central nervous system (CNS) drugs, such as pramipexole which is widely used for the treatment of Parkinson's disease. To evaluate the effectiveness of intranasal delivery of pramipexole, preclinical pharmacokinetic and tissue distribution studies following intranasal administration need to be investigated. In this paper, we developed and validated a robust and sensitive LC-MS/MS assay without matrix effect for accurate measurements of pramipexole in mouse plasma and tissue samples. Pramipexole and its stable isotope labeled internal standard (d3-pramipexole) were extracted from biological samples by protein precipitation (PPT) coupled with solid phase extraction (SPE) using weak cation exchange SPE cartridges. Matrix effects were studied using post-column infusion and post-extraction addition experiments by direct monitoring of typical phospholipids including glycerophosphocholines (GPChos) and lysoglycerophosphocholines (Lyso-GPChos). Chromatographic separation was achieved on a Welch Ultimate(®) XB-CN column using isocratic elution with a run time of 3.0 min. The assay was linear in the concentration range of 0.05-100 ng/mL and the intra- and inter-day precision and accuracy met the acceptance criteria. Compared with previous reported assays, the current sample preparation approach exhibited significant reduction of matrix effects due to the dramatically decreased levels of residual matrix components such as GPChos and Lyso-GPChos. This method has been successfully applied to pharmacokinetic and tissue distribution studies of pramipexole in mice following a single intravenous or intranasal dose of 50 μg/kg. PMID:25777479

  7. Selective determination of pharmaceuticals and illicit drugs in wastewaters using a novel strong cation-exchange solid-phase extraction combined with liquid chromatography-tandem mass spectrometry.

    PubMed

    Gilart, Núria; Cormack, P A G; Marcé, Rosa Maria; Fontanals, Núria; Borrull, Francesc

    2014-01-17

    In this study, two materials are presented with strong cation-exchange (SCX) behaviour synthesised by two different approaches and then crushed for their application as sorbents for solid-phase extraction (SPE) to extract a group of pharmaceuticals and illicit drugs selectively from wastewater samples. The first SCX polymer was obtained by copolymerisation of three monomers: 2-acrylamido-2-methylpropane sulphonic acid (AMPSA), 2-hydroxyethyl methacrylate (HEMA) and pentaerythritol triacrylate (PETRA), while the second was obtained by post-modification with sulphuric acid (H2SO4) of a copolymer based on HEMA and divinylbenzene (DVB). After their syntheses, both polymers were evaluated as SPE sorbents, with all parameters affecting SPE being optimised, such as sample pH, washing and elution solvents and volumes. Thanks to the sulphonic groups present in the structure of the polymers, all of the compounds with basic functionalities were retained on the sorbents after the washing step, removing the acidic analytes and other interfering compounds, providing successful results in terms of ion suppression/enhancement (-12% and 21%) when wastewater samples were analysed. However, AMPSA/HEMA/PETRA (20/60/20) failed to retain the analytes after loading wastewater samples (25 or 50mL), decreasing analyte recovery values significantly, whereas the sulphonated HEMA/DVB (50/50) enabled good SPE performance with recovery values between 70% and 98%, except for ranitidine and EDDP (39% and 43%, respectively). Therefore, this polymer was selected for further method validation and quantification of wastewater samples, providing low method detection limits (MDLs) in this matrix (from 2 to 40ngL(-1)). Finally, most of the studied compounds were detected and quantified in wastewater samples, especially atenolol, ranitidine, cocaine and its metabolite benzoylecgonine. PMID:24369996

  8. Elastic modulus of polypyrrole nanotubes: AFM measurement

    NASA Astrophysics Data System (ADS)

    Cuenot, Stéphane; Demoustier-Champagne, Sophie; Nysten, Bernard

    2001-03-01

    Polypyrrole nanotubes were electrochemically synthesized within the pores of nanoporous track-etched membranes. After dissolution of the template membrane, they were dispersed on PET membranes. Their tensile elastic modulus was measured by probing them in three points bending using an atomic force microscope. The elastic modulus was deduced from force-curve measurements. In this communication, the effect of the synthesis temperature and of the nanotube diameter will be presented. Especially it will be shown that the elastic modulus strongly increases when the nanotube outer diameter is reduced from 160 nm down to 35 nm. These results are in good agreement with previous results showing that the electrical conductivity of polypyrrole nanotubes increases by more than one order of magnitude when the diameter decreases in the same range. These behaviors could be explained by a larger ratio of well-oriented defect-free polymer chains in smaller tubes.

  9. Cuprous Ion Conducting Montmorillonite- Polypyrrole Nanocomposites

    NASA Astrophysics Data System (ADS)

    Krishantha, D. M. M.; Rajapakse, R. M. G.; Tennakoon, D. T. B.; Bandara, W. M. A. T.; Thilakarathna, P. N. L.

    2006-06-01

    Solid state polymer-Silicate nanocomposite based on Polypyrrole-Cu+-montmorilonite were prepared and electrical properties were investigated. In this preparation, Na-montmorillonite (Na+-MMT) was purified by repeated washing with distilled water and the intergallery cations were exchanged for Cu(II). The cupric ions exchanged-MMT(Cu(II)-- MMT) was again exposed to pyrrole in aqueous acidic solution to yield polypyrrole-Cu+-MMT nanocomposite. DC polarization test and AC impedance measurement reveal that the materials are mixed conductors. The ionic conductivity is due to the motion of cuprous ions which is facilitated by microstructure of polypyrrrole present in the intergalleries. An electrochemical cell was fabricated using the materials which can be represented by Cu(s)/ Cu+-PPY-MMT/Cu2SO4 (s)/Na2SO4(S)-Na2S2O8(s)/ and gave a 1.00 V. The cell is rechargeable.

  10. Adhesion of Particulate Materials to Mesostructured Polypyrrole

    NASA Astrophysics Data System (ADS)

    Hoss, Darby; Knepper, Robert; Hotchkiss, Peter; Tappan, Alexander; Boudouris, Bryan; Beaudoin, Stephen

    Interactions based on van der Waals (vdW) forces will influence the performance and reliability of mesostructured polypyrrole swabs used for the collection and detection of trace particles. The vdW adhesion force between materials is described by the Hamaker constant, and these constants are measured via optical and dielectric properties (i.e., according to Lifshitz theory), inverse gas chromatography (IGC), and contact angle measurements. Here, contact angle measurements were performed on films of several common materials and used to estimate Hamaker constants. This, in turn, will allow for the tuning of the design properties associated with the polypyrrole swabs. A comparison of these results to Hamaker constants estimated using Lifshitz Theory and IGC reveals the fundamental behavior of the materials. The Hamaker constants were then used in a new computational vdW adhesion model. The idealized model describes particle adhesion to an array of mesostrucures. This model elucidates the importance of where the particle makes contact with the mesostructure and the independence of vdW forces generated by each mesostructure. These results will facilitate the rational design of polypyrrole swabs optimized for harvesting microscale particles of trace materials.

  11. Novel Preparation of Nano-Composite CuO-Cr2O3 Using Ctab-Template Method and Efficient for Hydrogenation of Biomass-Derived Furfural

    NASA Astrophysics Data System (ADS)

    Yan, Kai; Wu, Xu; An, Xia; Xie, Xianmei

    2013-02-01

    A simple route to fabricate nano-composite oxides CuO-Cr2O3 using hexadecyltrimethylammonium bromide (CTAB)-templated Cu-Cr hydrotalcite as the precursor is presented. This novel method is based on CTAB-templating effect for mesostructure directing and using the cheap metal nitrate, followed by removal of CTAB. It was indicated that the nano-composite CuO-Cr2O3 was formed during the removal of CTAB. X-ray diffraction (XRD) and transitional electronic microscopy (TEM) revealed nice nano-composite oxides CuO-Cr2O3 were formed with high crystallinity. N2 adsorption and desorption indicated that a high surface area of 170.5 m2/g with a pore size of 2.7 nm of the nano-composite CuO-Cr2O3 was facilely resulted. The as-synthesized nano-composite oxides CuO-Cr2O3 display good catalytic activities for hydrogenation of furfural to furfuryl alcohol, whereas 86% selectivity was achieved at 75% conversion of furfural.

  12. Tandem anion and cation exchange solid phase extraction for the enrichment of micropollutants and their transformation products from ozonation in a wastewater treatment plant.

    PubMed

    Deeb, Ahmad A; Schmidt, Torsten C

    2016-06-01

    The presence of organic micropollutants and their transformation products (TPs) from biotic and abiotic processes in aquatic environments is receiving intense public and scientific attention. Yet a suitable sample preparation method that would enable extraction and enrichment of a wide range of such compounds from water is missing. The focus of this paper was to develop an enhanced solid phase extraction (SPE) protocol which enabled isolation of parent compounds and low molecular weight transformation products (that are produced after treatment of water with ozone) from different water matrices. Ten SPE sorbents were evaluated with regard to their ability to extract acidic, neutral, and basic compounds from water at several pH values. Highest recoveries (91-99 %) for all analytes in pure water were obtained by combining strong anion and cation exchangers of two manufacturers in a tandem mode without pH adjustment. Tandem Oasis (MAX+MCX) was finally applied to extract the spiked analytes from tap water, surface water, and several wastewater samples. The efficiency of the used SPE procedure was examined using an optimized liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) method using multiple reaction monitoring (MRM) mode. The occurrence of some of the investigated TPs in environmental water matrices was proven for the first time in this study. Method quantification limits (MQLs) for all compounds ranged from 3.7 to 15.3 ng/L in all matrices. Recoveries (%RE) were between 90 and 110 %. Intraday and interday precision, expressed as relative standard deviation, varied from 0.7 to 5.9 % and 1.8 to 10.3 %, respectively. Matrix effect (%ME) evaluation demonstrated that even complex sample matrices did not show significant ion suppression or enhancement. The applicability of the method was shown during two sampling campaigns at Ruhr river and a wastewater treatment plant (WWTP) equipped with an ozonation step after regular

  13. Applying reactive models to column experiments to assess the hydrogeochemistry of seawater intrusion: Optimising ACUAINTRUSION and selecting cation exchange coefficients with PHREEQC

    NASA Astrophysics Data System (ADS)

    Boluda-Botella, N.; Valdes-Abellan, J.; Pedraza, R.

    2014-03-01

    Three sets of laboratory column experimental results concerning the hydrogeochemistry of seawater intrusion have been modelled using two codes: ACUAINTRUSION (Chemical Engineering Department, University of Alicante) and PHREEQC (U.S.G.S.). These reactive models utilise the hydrodynamic parameters determined using the ACUAINTRUSION TRANSPORT software and fit the chloride breakthrough curves perfectly. The ACUAINTRUSION code was improved, and the instabilities were studied relative to the discretisation. The relative square errors were obtained using different combinations of the spatial and temporal steps: the global error for the total experimental data and the partial error for each element. Good simulations for the three experiments were obtained using the ACUAINTRUSION software with slight variations in the selectivity coefficients for both sediments determined in batch experiments with fresh water. The cation exchange parameters included in ACUAINTRUSION are those reported by the Gapon convention with modified exponents for the Ca/Mg exchange. PHREEQC simulations performed using the Gains-Thomas convention were unsatisfactory, with the exchange coefficients from the database of PHREEQC (or range), but those determined with fresh water - natural sediment allowed only an approximation to be obtained. For the treated sediment, the adjusted exchange coefficients were determined to improve the simulation and are vastly different from those from the database of PHREEQC or batch experiment values; however, these values fall in an order similar to the others determined under dynamic conditions. Different cation concentrations were simulated using two different software packages; this disparity could be attributed to the defined selectivity coefficients that affect the gypsum equilibrium. Consequently, different calculated sulphate concentrations are obtained using each type of software; a smaller mismatch was predicted using ACUAINTRUSION. In general, the presented

  14. Weak cation exchange magnetic beads coupled with matrix-assisted laser desorption ionization-time of flight-mass spectrometry in screening serum protein markers in osteopenia.

    PubMed

    He, Wei-Tao; Liang, Bo-Cheng; Shi, Zhen-Yu; Li, Xu-Yun; Li, Chun-Wen; Shi, Xiao-Lin

    2016-01-01

    The present study aimed at investigating the weak cation magnetic separation technology and matrix-assisted laser desorption ionization-time of flight-mass spectrometry (MALDI-TOF-MS) in screening serum protein markers of osteopenia from ten postmenopausal women and ten postmenopausal women without osteopenia as control group, to find a new method for screening biomarkers and establishing a diagnostic model for primary type I osteoporosis. Serum samples were collected from postmenopausal women with osteopenia and postmenopausal women with normal bone mass. Proteins were extracted from serum samples by weak cation exchange magnetic beads technology, and mass spectra acquisition was done by MALDI-TOF-MS. The visualization and comparison of data sets, statistical peak evaluation, model recognition, and discovery of biomarker candidates were handled by the proteinchip data analysis system software(ZJU-PDAS). The diagnostic models were established using genetic arithmetic based support vector machine (SVM). The SVM result with the highest Youden Index was selected as the model. Combinatorial Peaks having the highest accuracy in distinguishing different samples were selected as potential biomarker. From the two group serum samples, a total of 133 differential features were selected. Ten features with significant intensity differences were screened. In the pair-wise comparisons, processing of MALDI-TOF spectra resulted in the identification of ten differential features between postmenopausal women with osteopenia and postmenopausal women with normal bone mass. The difference of features by Youden index showed that the highest features had a mass to charge ratio of 1699 and 3038 Da. A diagnosis model was established with these two peaks as the candidate marker, and the specificity of the model is 100 %, the sensitivity was 90 % by leave-one-out cross validation test. The two groups of specimens in SVM results on the scatter plot could be clearly distinguished. The peak

  15. Fabrication of lotus-leaf-like superhydrophobic surfaces via Ni-based nano-composite electro-brush plating

    NASA Astrophysics Data System (ADS)

    Liu, Hongtao; Wang, Xuemei; Ji, Hongmin

    2014-01-01

    Superhydrophobic surface has become a research hot topic in recent years due to its excellent performance and wide application prospect. This paper investigates the method to fabricate superhydrophobic surface on carbon steel substrate via two-layer nano-composite electro-brush plating and subsequent surface modification with low free energy materials. The hydrophobic properties of as-prepared coatings were characterized by a water sliding angle (SA) and a water contact angle (CA) measured by the Surface tension instrument. A Scanning electron microscope was used to analyze the surface structure of plating coatings. Anti-corrosion performance of the superhydrophobic coating was characterized by a potentiodynamic polarization curve measured by the Electrochemical workstation. The research result shows that: the superhydrophobic structure can be successfully prepared by plating nano-C/Ni and nano-Cu/Ni two-layer coating on carbon steel substrate under appropriate technology and has similarity with lotus-leaf-like micro/nano composite structure; the contact angle of the as-prepared superhydrophobic coating can be up to 155.5°, the sliding angle is 5°; the coating has better anti-corrosion performance compared with substrate.

  16. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor.

    PubMed

    Jomma, Ezzaldeen Younes; Ding, Shou-Nian

    2016-01-01

    In this work, we presented a simple method to synthesize magnetite Prussian blue nano-composites (Fe₃O₄-PB) through one-pot hydrothermal process. Subsequently, the obtained nano-composites were used to fabricate a facile and effective glucose biosensor. The obtained nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, Fourier-transform infrared spectroscopy, UV-vis absorbance spectroscopy, cyclic voltammetry and chronoamperometry. The resultant Fe₃O₄-PB nanocomposites have magnetic properties which could easily controlled by an external magnetic field and the electro-catalysis of hydrogen peroxide. Thus, a glucose biosensor based on Fe₃O₄-PB was successfully fabricated. The biosensor showed super-electrochemical properties toward glucose detection exhibiting fast response time within 3 to 4 s, low detection limit of 0.5 µM and wide linear range from 5 µM to 1.2 mM with sensitivity of 32 µA∙mM(-1)∙cm(-2) and good long-term stability. PMID:26901204

  17. TiO2 micro/nano-composite structured electrodes for quasi-solid-state dye-sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Zhao, Yong; Zhai, Jin; Tan, Shuxin; Wang, Lifang; Jiang, Lei; Zhu, Daoben

    2006-05-01

    Micro/nano-composite TiO2 porous films are prepared in a nutshell by the electro-hydrodynamic (EHD) method, and are applied to dye sensitized solar cells (DSSCs) successfully. Considering that micro/nano-composite structures based on the EHD technique are better for the filling of ionic liquid and quasi-solid-state electrolytes than liquid state electrolytes, a fill factor (ff) of 78.9% and a total photoelectric conversion efficiency (η) of 6.4% for ionic liquid electrolyte and an ff of 75.3% and an η of 5.3% for quasi-solid-state electrolyte are obtained. Moreover, this kind of composite hierarchical structure may be of benefit for light collection because of strong light scattering. In order to obtain optimized devices, we probe into the influence of adding an amount of polymer on the photovoltaic performance, and find that by changing the concentration of the polymer during the EHD process the specific surface area of the films changes, which leads to different photovoltaic behaviour of solar cells.

  18. One-Pot Hydrothermal Synthesis of Magnetite Prussian Blue Nano-Composites and Their Application to Fabricate Glucose Biosensor

    PubMed Central

    Jomma, Ezzaldeen Younes; Ding, Shou-Nian

    2016-01-01

    In this work, we presented a simple method to synthesize magnetite Prussian blue nano-composites (Fe3O4-PB) through one-pot hydrothermal process. Subsequently, the obtained nano-composites were used to fabricate a facile and effective glucose biosensor. The obtained nanoparticles were characterized using transmission electron microscopy, scanning electron microscopy, Fourier-transform infrared spectroscopy, UV-vis absorbance spectroscopy, cyclic voltammetry and chronoamperometry. The resultant Fe3O4-PB nanocomposites have magnetic properties which could easily controlled by an external magnetic field and the electro-catalysis of hydrogen peroxide. Thus, a glucose biosensor based on Fe3O4-PB was successfully fabricated. The biosensor showed super-electrochemical properties toward glucose detection exhibiting fast response time within 3 to 4 s, low detection limit of 0.5 µM and wide linear range from 5 µM to 1.2 mM with sensitivity of 32 µA∙mM−1∙cm−2 and good long-term stability. PMID:26901204

  19. Au-C allotrope nano-composite films at extreme conditions generated by intense ultra-short laser

    NASA Astrophysics Data System (ADS)

    Khan, Saif A.; Saravanan, K.; Tayyab, M.; Bagchi, S.; Avasthi, D. K.

    2016-07-01

    Structural evolution of gold-carbon allotrope nano-composite films under relativistically intense, ultra-short laser pulse irradiation is studied in this work. Au-C nano-composite films, having 4 and 10 at.% of Au, were deposited by co-sputtering technique on silicon substrates. Au-C60 NC films with 2.5 at.% Au were deposited on 12 μm thick Al foil using co-evaporation technique. These samples were radiated with single pulse from 45 fs, 10 TW Ti:Sapphire Laser at RRCAT at an intensity of 3 × 1018 W cm-2. The morphological and compositional changes were investigated using scanning electron microscopy (SEM) and Rutherford back-scattering spectrometry (RBS) techniques. Laser pulse created three morphologically distinct zones around the point of impact on samples with silicon substrates. The gold content in 600 μm circular region around a point of impact is found to reduce by a factor of five. Annular rings of ∼70 nm in diameter were observed in case of Au-C NC film after irradiation. Laser pulse created a hole of about 400 μm in the sample with Al foil as substrate and wavy structures of 6 μm wavelength are found to be created around this hole. The study shows radial variation in nano-structure formation with varying local intensity of laser pulse.

  20. Synthesis of TiB2-TiC/Fe nano-composite coating by laser surface engineering

    NASA Astrophysics Data System (ADS)

    Du, Baoshuai; Paital, Sameer R.; Dahotre, Narendra B.

    2013-02-01

    The study explores the synthesis of TiB2 and TiC reinforced Fe-based nano-composite coating by laser surface engineering using Ti, B4C and Fe powder mixture as precursor. The effect of laser scanning speed on the size, morphology, and amount of nano-sized ceramic reinforcements were studied at laser fluence of 1111 J/cm2, 1667 J/cm2 and 3333 J/cm2 respectively. A bimodal microstructure with TiC and TiB2 particles dispersed in fine α-Fe matrix was evolved in the laser processed coatings. Besides, the nature of formation of nano-sized ceramic phase was examined. The laser synthesized nano-composite coating yielded 3-5 times increase in microhardness. It appears that the presence of nano-sized TiB2 and TiC particles coupled with the highly refined α-Fe matrix improves the hardness significantly. This coating offers the potential to increase the hardness and toughness simultaneously for developing wear-resistance coatings.

  1. Study on the resistance performance of TiO2/cyanate ester nano-composites exposed to electron radiation

    NASA Astrophysics Data System (ADS)

    Qin, Wei; Peng, Dequn; Wu, Xiaohong; Liao, Junhai

    2014-04-01

    TiO2 nano-particles were incorporated into cyanate ester (CE) resin to form TiO2/CE nano-composites. The effects of electron radiation on CE resin and on TiO2/CE nano-composites were investigated in a ground-based simulator that simulates space radiation conditions. Compared with CE resin, the addition of TiO2 nano-particles to the CE resin increased the bend strength and it improved the toughness before and after the electron radiation. The electron radiation damage mainly occurred in the CE resin matrix. The electric discharging resulted in the ablation of the CE resin surface when the charges were cumulated to a certain extent. The results of the mass loss and infrared (IR) experiments indicated that the electron irradiation in high vacuum broke the surface chemical bonds and that a cross-linking process occurred in the surface layer. The results of the electron paramagnetic resonance (EPR) showed that nano-TiO2 particles contribute a better resistance performance under 160-keV electron radiation.

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

    PubMed

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

    2015-05-15

    Present study deals with the preparation and evaluation of graphene based magnetic nano-composite for dispersive solid phase extraction of Chemical Weapons Convention (CWC) relevant chemicals from aqueous samples. Nano-composite, Fe3O4@SiO2-G was synthesized by covalently bonding silica coated Fe3O4 onto the graphene sheets. Nerve agents (NA), Sulfur mustard (SM) and their non-toxic environmental markers were the target analytes. Extraction parameters like amount of sorbent, extraction time and desorption conditions were optimized. Dispersion of 20 milligram of sorbent in 200mL of water sample for 20min. followed by methanol/chloroform extraction produced average to good recoveries (27-94%) of targeted analytes. Recoveries of real agents exhibited great dependency upon sample pH and ionic strength. Sarin produced maximum recovery under mild acidic conditions (56% at pH 5) while VX demanded alkaline media (83% at pH 9). Salts presence in the aqueous samples was found to be advantageous, raising the recoveries to as high as 94% for SM. Excellent limits of detection (LOD) for sulphur mustard and VX (0.11ngmL(-1) and 0.19ngmL(-1) respectively) proved the utility of the developed method for the off-site analysis of CWC relevant chemicals. PMID:25828545

  3. Novel nano-composite biomimetic biomaterial allows chondrogenic and osteogenic differentiation of bone marrow concentrate derived cells.

    PubMed

    Grigolo, Brunella; Cavallo, Carola; Desando, Giovanna; Manferdini, Cristina; Lisignoli, Gina; Ferrari, Andrea; Zini, Nicoletta; Facchini, Andrea

    2015-04-01

    In clinical orthopedics suitable materials that induce and restore biological functions together with the right mechanical properties are particularly needed for the regeneration of osteochondral lesions. For this purpose, the ideal scaffold should possess the right properties with respect to degradation, cell binding, cellular uptake, non-immunogenicity, mechanical strength, and flexibility. In addition, it should be easy to handle and serve as a template for chondrocyte and bone cells guiding both cartilage and bone formation. The aim of the present study was to estimate the chondrogenic and osteogenic capability of bone marrow concentrated derived cells seeded onto a novel nano-composite biomimetic material. These properties have been evaluated by means of histological, immunohistochemical and electron microscopy analyses. The data obtained demonstrated that freshly harvested cells obtained from bone marrow were able, once seeded onto the biomaterial, to differentiate either down the chondrogenic and osteogenic pathways as evaluated by the expression and production of specific matrix molecules. These findings support the use, for the repair of osteochondral lesions, of this new nano-composite biomimetic material together with bone marrow derived cells in a "one step" transplantation procedure. PMID:25804305

  4. Digital selective fabrication of micro/nano-composite structured TiO2 nanorod arrays by laser direct writing

    NASA Astrophysics Data System (ADS)

    Jiang, Wei; He, Xiaoning; Liu, Hongzhong; Yin, Lei; Shi, Yongsheng; Ding, Yucheng

    2014-11-01

    In this article, we report on the digital selective fabrication of micro/nano-composite structured TiO2 nanorod arrays by laser direct writing. The pattern of TiO2 nanorod arrays can be easily designed and fabricated by laser scanning technology integrated with a computer-aided design system, which allows a high degree of freedom corresponding to the various pattern design demands. The approach basically involves the hydrothermal growth of TiO2 nanorod arrays on a transparent conductive substrate, the micropattern of TiO2 nanorod arrays and surface fluorination treatment. With these micro/nano-composite TiO2 nanorod array based films, we have demonstrated superhydrophilic patterned TiO2 nanorod arrays with rapid water spreading ability and superhydrophobic patterned TiO2 nanorod arrays with an excellent droplet bouncing effect and a good self-cleaning performance. The dynamic behaviours of the water droplets observed on the patterned TiO2 nanorod arrays were demonstrated by experiments and simulated by a finite element method. The approaches we will show are expected to provide potential applications in fields such as self-cleaning, surface protection, anticrawling and microfluidic manipulation.

  5. Electrochemical biosensing based on polypyrrole/titania nanotube hybrid.

    PubMed

    Xie, Yibing; Zhao, Ye

    2013-12-01

    The glucose oxidase (GOD) modified polypyrrole/titania nanotube enzyme electrode is fabricated for electrochemical biosensing application. The titania nanotube array is grown directly on a titanium substrate through an anodic oxidation process. A thin film of polypyrrole is coated onto titania nanotube array to form polypyrrole/titania nanotube hybrid through a normal pulse voltammetry process. GOD-polypyrrole/titania nanotube enzyme electrode is prepared by the covalent immobilization of GOD onto polypyrrole/titania nanotube hybrid via the cross-linker of glutaraldehyde. The morphology and microstructure of nanotube electrodes are characterized by field emission scanning electron microscopy and Fourier transform infrared analysis. The biosensing properties of this nanotube enzyme electrode have been investigated by means of cyclic voltammetry and chronoamperometry. The hydrophilic polypyrrole/titania nanotube hybrid provides highly accessible nanochannels for GOD encapsulation, presenting good enzymatic affinity. As-formed GOD-polypyrrole/titania nanotube enzyme electrode well conducts bioelectrocatalytic oxidation of glucose, exhibiting a good biosensing performance with a high sensitivity, low detection limit and wide linear detection range. PMID:24094220

  6. Electrodeposition of Copper onto Polypyrrole Films: Application to Proton Reduction

    NASA Astrophysics Data System (ADS)

    Chikouche, Imene; Sahari, Ali; Zouaoui, Ahmed; Zegadi, Ameur

    2016-09-01

    In this paper, we have electrodeposited copper on polypyrrole surface. Results show that at high applied cathodic potential (>-1.8V), copper electrodeposition occurs with difficulties. The amount of electrodeposited copper is low (1.32%) and it is limited by the low polypyrrole conductivity. At this potential, poor conductivity is caused by its insulating state. However, at an applied cathodic potential of -1.2V, the polypyrrole exhibits a relatively high conductivity and copper particles are electrodeposited with large amounts (12.44%) on polypyrrole/silicon system. At high applied cathodic potential, the SEM images show clearly dispersed grains of copper, but polypyrrole surface is less occupied. At an applied cathodic potential of -1.2V, the SEM image shows that polypyrrole surface is homogenously more occupied with copper. After copper deposition, the Cu/PPy/Si system is used to catalyze the hydrogen reaction. It was found that, once the deposited copper is present with considerable amounts, the proton reduction occurs easily. As for the polypyrrole conductivity, it was found that electrodeposited copper onto PPy/Si surface affect the total conductivity.

  7. Impedance spectra of polypyrrole coated platinum electrodes.

    PubMed

    Onnela, Niina; Savolainen, Virpi; Hiltunen, Maiju; Kellomäki, Minna; Hyttinen, Jari

    2013-01-01

    Polypyrrole (PPy) coated electrodes may provide new solutions to increase the charge injection capacity and biocompatibility of metal electrodes in e.g., neural stimulus applications. In this study, electrical impedance spectra of PPy coated platinum (Pt) electrodes having three different coating thicknesses were measured and modeled. A suitable equivalent electrical circuit providing the material characteristics was chosen and the impedance data was analyzed using the model and data fitting. The modeled parameter values of different coating thicknesses were compared and our results demonstrated the changes in charge transfer properties and mechanisms of thin and thick PPy film coatings. PMID:24109743

  8. Vanadium oxide/polypyrrole aerogel nanocomposites

    SciTech Connect

    Dave, B.C.; Dunn, B.S.; Wong, H.P.; Leroux, F.; Nazar, L.F.

    1996-12-31

    Vanadium pentoxide/polypyrrole aerogel (ARG) nanocomposites were prepared by hydrolysis of VO(OC{sub 3}H{sub 7}){sub 3} using pyrrole/water/acetone mixtures. Monolithic green-black gels with polypyrrole/V ratios ranging from 0.15 to 1.0 resulted from simultaneously polymerization of the pyrrole and vanadium alkoxide precursors. Supercritical drying yielded high surface (150--200 m{sup 2}/g) aerogels, of sufficient mechanical integrity to allow them to be cut without fracturing. TEM studies of the aerogels show that they are comprised of fibers similar to that of V{sub 2}O{sub 5} ARG`s, but with a much shorter chain length. Evidence from IR that the inorganic and organic components strongly interact leads them to propose that this impedes the vanadium condensation process. The result is ARG`s that exhibit decreased electronic conductivity with increasing polymer content. Despite the unexpected deleterious effect of the conductive polymer on the bulk conductivity, at low polymer content, the nanocomposite materials show enhanced electrochemical properties for Li insertion compared to the pristine aerogel.

  9. Graphene nano-devices and nano-composites for structural, thermal and sensing applications

    NASA Astrophysics Data System (ADS)

    Yavari, Fazel

    In this dissertation we have developed graphene-based nano-devices for applications in integrated circuits and gas sensors; as well as graphene-based nano-composites for applications in structures and thermal management. First, we have studied the bandgap of graphene for semiconductor applications. Graphene as a zero-bandgap material cannot be used in the semiconductor industry unless an effective method is developed to open the bandgap in this material. We have demonstrated that a bandgap of 0.206 eV can be opened in graphene by adsorption of water vapor molecules on its surface. Water molecules break the molecular symmetries of graphene resulting in a significant bandgap opening. We also illustrate that the lack of bandgap in graphene can be used to our advantage by making sensors that are able to detect low concentrations of gas molecules mixed in air. We have shown that 1-2 layers of graphene synthesized by chemical vapor deposition enables detection of trace amounts of NO 2 and NH3 in air at room temperature and atmospheric pressure. The gas species are detected by monitoring changes in electrical resistance of the graphene film due to gas adsorption. The sensor response time is inversely proportional to the gas concentration. Heating the film expels chemisorbed molecules from the graphene surface enabling reversible operation. The detection limits of ~100 parts-per-billion (ppb) for NO2 and ~500 ppb for NH3 obtained using this device are markedly superior to commercially available NO2 and NH3 detectors. This sensor is fabricated using individual graphene sheets that are exquisitely sensitive to the chemical environment. However, the fabrication and operation of devices that use individual nanostructures for sensing is complex, expensive and suffers from poor reliability due to contamination and large variability from sample-to-sample. To overcome these problems we have developed a gas sensor based on a porous 3D network of graphene sheets called graphene foam

  10. Graphene nano-devices and nano-composites for structural, thermal and sensing applications

    NASA Astrophysics Data System (ADS)

    Yavari, Fazel

    In this dissertation we have developed graphene-based nano-devices for applications in integrated circuits and gas sensors; as well as graphene-based nano-composites for applications in structures and thermal management. First, we have studied the bandgap of graphene for semiconductor applications. Graphene as a zero-bandgap material cannot be used in the semiconductor industry unless an effective method is developed to open the bandgap in this material. We have demonstrated that a bandgap of 0.206 eV can be opened in graphene by adsorption of water vapor molecules on its surface. Water molecules break the molecular symmetries of graphene resulting in a significant bandgap opening. We also illustrate that the lack of bandgap in graphene can be used to our advantage by making sensors that are able to detect low concentrations of gas molecules mixed in air. We have shown that 1-2 layers of graphene synthesized by chemical vapor deposition enables detection of trace amounts of NO 2 and NH3 in air at room temperature and atmospheric pressure. The gas species are detected by monitoring changes in electrical resistance of the graphene film due to gas adsorption. The sensor response time is inversely proportional to the gas concentration. Heating the film expels chemisorbed molecules from the graphene surface enabling reversible operation. The detection limits of ~100 parts-per-billion (ppb) for NO2 and ~500 ppb for NH3 obtained using this device are markedly superior to commercially available NO2 and NH3 detectors. This sensor is fabricated using individual graphene sheets that are exquisitely sensitive to the chemical environment. However, the fabrication and operation of devices that use individual nanostructures for sensing is complex, expensive and suffers from poor reliability due to contamination and large variability from sample-to-sample. To overcome these problems we have developed a gas sensor based on a porous 3D network of graphene sheets called graphene foam

  11. Structural, morphological and optical properties of PEDOT:PSS/QDs nano-composite films prepared by spin-casting

    NASA Astrophysics Data System (ADS)

    Najeeb, Mansoor Ani; Abdullah, Shahino Mah; Aziz, Fakhra; Ahmad, Zubair; Rafique, Saqib; Wageh, S.; Al-Ghamdi, Ahmed A.; Sulaiman, Khaulah; Touati, Farid; Shakoor, R. A.; Al-Thani, N. J.

    2016-09-01

    This paper describes the structural, morphological and optical properties of the nano-composite of poly (3,4-ethylenedioxythiophene) polystyrene sulfonate (PEDOT:PSS) and quantum dots (QDs). The ZnSe and CdSe QDs have been synthesized, with the aid of Mercaptoacetic acid (MAA), by a colloidal method with an average size of ~5 to 7 nm. QDs have been embedded in PEDOT:PSS using a simple solution processing approach and has been deposited as thin films by spin coating technique. The QDs embedded PEDOT:PSS enhances the light absorption spectra of samples, prominently in terms of absorption intensity which may consequently improve sensitivity of the optoelectronic devices.

  12. Immobilization of laccase on a novel ZnO/SiO2 nano-composited support for dye decolorization

    NASA Astrophysics Data System (ADS)

    Li, Wei-Xun; Sun, Huai-Yan; Zhang, Rui-Feng

    2015-07-01

    ZnO nanowires were introduced into macroporous SiO2 by means of in situ hydrothermal growth. The obtained nano-composite was then used to immobilize laccase (secured from Trametes versicolor) through the process of static adsorption. The average loading amount was as high as 193.4 μmol-g-1. The immobilized laccase was proven to be an effective biocatalyst in the decolorization of two dyes: Remazol Brilliant Blue B, and Acid Blue 25. The decolorization percentage of Remazol Brilliant Blue B and Acid Blue 25 reached 93% and 82% respectively. The immobilized laccase exhibited enhanced thermal stability and pH adaptability compared to free laccase. After ten recycles, the immobilized laccase retained 42% decolorization catalytic activity.

  13. Influence of Process Control Agents on Mechanochemical Synthesis of NiAl/Al2O3 Nano Composite powder

    NASA Astrophysics Data System (ADS)

    Heshmati-Manesh, S.; Jabbarnia, A.

    2010-03-01

    Mechanochemical synthesis of an intermetallic NiAl matrix nano composite powder has been studied in this paper. Micron sized powders of nickel oxide (NiO) and aluminum powders were subjected to high energy ball milling under an argon protected atmosphere. According to an exothermic exchange reaction assisted by high energy ball milling, nickel oxide is reduced by Al and a NiAl/Al2O3 composite powder is produced. The process was also examined when stearic acid and methanol were added as process control agents (PCAs) to the reactants and it was found that their addition hinders the reduction reaction. The effect of further milling on the milling behavior of the resulting composite powder has also been investigated. The morphology and phase composition of the milling products were evaluated by scanning electron microscopy (SEM) and X-ray diffraction (XRD) analysis.

  14. Co and Cu co-doped ZnO epitaxial films—A magnetically soft nano-composite

    NASA Astrophysics Data System (ADS)

    Ney, V.; Venkataraman, V.; Henne, B.; Ollefs, K.; Wilhelm, F.; Rogalev, A.; Ney, A.

    2016-04-01

    A series of Co/Cu co-doped ZnO epitaxial films has been grown on sapphire substrates to investigate the possibilities of tailoring the magnetic properties in functional ZnO-Co/Cu nano-composites. The growth was performed using reactive magnetron sputtering varying the oxygen partial pressure to tune the incorporation of the dopants and the resulting valence state. At high oxygen pressures, Co2+ is formed and the resulting magnetic properties are very similar to phase pure paramagnetic Co-doped ZnO samples. However, the formation of a secondary CuO phase reduces the overall structural quality of the layers and virtually no substitutional incorporation of Cu2+ in ZnO could be evidenced. At low oxygen pressures, a significant fraction of metallic Co and Cu forming nanometer-sized superparamagnetic precipitates of a Co/Cu alloy can be evidenced which are embedded in a ZnO host matrix.

  15. Synthesis and Characterization of Polypyrrole Coated SBR Composites

    NASA Astrophysics Data System (ADS)

    Mathew, Anisha Mary; Neena, P.; Prasanth, S.; Panwar, N. S.; Pradeep, P.

    2008-04-01

    Conducting polymer of styrene butadiene rubber has been synthesized by chemical doping method. Subsequently the samples were coated with an intrinsically conducting polymer shell (ICP) of polypyrrole. The polymer shell was synthesized by chemical route method after the preparation of conducting polymer powder of SBR. The chemical structure of the composite was analyzed by taking the FTIR spectra. Electrical conductivity of the new hybrid material is found to be same as the conductivity of polypyrrole.

  16. Microstructuring of polypyrrole by maskless direct femtosecond laser ablation.

    PubMed

    Lee, Kenneth K C; Herman, Peter R; Shoa, Tina; Haque, Moez; Madden, John D W; Yang, Victor X D

    2012-03-01

    Ultrafast laser micromachining was optimized for microstructuring polypyrrole as a facile new approach towards tailoring electrochemical and mechanical responses desirable for microactuator, sensors, neural probing, and nerve conduit applications. Laser perforation of high-density and high aspect ratio through-holes generated greater than 5-fold increase in surface area. The flexible machining technique offers micron-size resolution and fast prototyping capability for optimizing properties and opening new directions for polypyrrole-based devices. PMID:22290691

  17. Porous vitalium-base nano-composite for bone replacement: Fabrication, mechanical, and in vitro biological properties.

    PubMed

    Dehaghani, Majid Taghian; Ahmadian, Mehdi

    2016-04-01

    Porous nano-composites were successfully prepared on addition of 58S bioactive glass to Co-base alloy with porosities of 37.2-58.8% by the combination of milling, space-holder and powder metallurgy techniques. The results of X-ray diffraction analysis showed that induced strain during milling of the Co-base alloy powder and also isothermal heat treatment during sintering process led to HCP↔FCC phase transformation which affected mechanical properties of the samples during compression test. Field emission scanning electron microscopy images showed that despite the remaining 58S powder in nanometer size in the composite, there were micro-particles due to sintering at high temperature which led to two different apatite morphologies after immersion in simulated body fluid. Calculated elastic modulus and 0.2% proof strength from stress-strain curves of compression tests were in the range of 2.2-8.3GPa and 34-198MPa, respectively. In particular, the mechanical properties of sample with 37.2% were found to be similar to those of human cortical bone. Apatite formation which was identified by scanning electron microscopy (SEM), pH meter and Fourier-transform infrared spectroscopy (FTIR) analysis showed that it could successfully convert bioinert Co-base alloy to bioactive type by adding 58S bioglass nano-particles. SEM images of cell cultured on the porous nano-composite with 37.2% porosity showed that cells properly grew on the surface and inside the micro and macro-pores. PMID:26874088

  18. Effect of gamma radiation and accelerated aging on the mechanical and thermal behavior of HDPE/HA nano-composites for bone tissue regeneration

    PubMed Central

    2013-01-01

    Background The replacement of hard tissues demands biocompatible and sometimes bioactive materials with properties similar to those of bone. Nano-composites made of biocompatible polymers and bioactive inorganic nano particles such as HDPE/HA have attracted attention as permanent bone substitutes due to their excellent mechanical properties and biocompatibility. Method The HDPE/HA nano-composite is prepared using melt blending at different HA loading ratios. For evaluation of the degradation by radiation, gamma rays of 35 kGy, and 70 kGy were used to irradiate the samples at room temperature in vacuum. The effects of accelerated ageing after gamma irradiation on morphological, mechanical and thermal properties of HDPE/HA nano-composites were measured. Results In Vitro test results showed that the HDPE and all HDPE/HA nano-composites do not exhibit any cytotoxicity to WISH cell line. The results also indicated that the tensile properties of HDPE/HA nano-composite increased with increasing the HA content except fracture strain decreased. The dynamic mechanical analysis (DMA) results showed that the storage and loss moduli increased with increasing the HA ratio and the testing frequency. Finally, it is remarked that all properties of HDPE/HA is dependent on the irradiation dose and accelerated aging. Conclusion Based on the experimental results, it is found that the addition of 10%, 20% and 30% HA increases the HDPE stiffness by 23%, 44 and 59% respectively. At the same time, the G’ increased from 2.25E11 MPa for neat HDPE to 4.7E11 MPa when 30% HA was added to the polymer matrix. Also, significant improvements in these properties have been observed due to irradiation. Finally, the overall properties of HDPE and its nano-composite properties significantly decreased due to aging and should be taken into consideration in the design of bone substitutes. It is attributed that the developed HDPE/HA nano-composites could be a good alternative material for bone tissue

  19. Novel silicon carbide/polypyrrole composites; preparation and physicochemical properties

    SciTech Connect

    Omastova, Maria . E-mail: upolmaom@savba.sk; Boukerma, Kada; Chehimi, Mohamed M.; Trchova, Miroslava

    2005-05-18

    Novel silicon carbide/polypyrrole (SiC/PPy) conducting composites were prepared using silicon carbide as inorganic substrate. The surface modification of SiC was performed in aqueous solution by oxidative polymerization of pyrrole using ferric chloride as oxidant. Elemental analysis was used to determine the mass loading of polypyrrole in the SiC/PPy composites. Scanning electron microscopy showed the surface modification of SiC by PPy. PPy in composites was confirmed by the presence of PPy bands in the infrared spectra of SiC/PPy containing various amounts of conducting polymer. The conductivity of SiC/PPy composites depends on PPy content on the surface. The composite containing 35 wt.% PPy showed conductivity about 2 S cm{sup -1}, which is in the same range as the conductivity of pure polypyrrole powder prepared under the same conditions using the same oxidant. PPy in the composites was clearly detected by X-ray photoelectron spectroscopy (XPS) measurements by its N1s and Cl2p peaks. High resolution scans of the C1s regions distinguished between silicon carbide and polypyrrole carbons. The fraction of polypyrrole at the composite surface was estimated from the silicon and nitrogen levels. The combination of XPS and conductivity measurements suggests that the surface of the SiC/PPy composites is polypyrrole-rich for a conducting polymer mass loading of at least 12.6 wt.%.

  20. LPG ammonia and nitrogen dioxide gas sensing properties of nanostructured polypyrrole thin film

    NASA Astrophysics Data System (ADS)

    Bagul, Sagar B.; Upadhye, Deepak S.; Sharma, Ramphal

    2016-05-01

    Nanostructured Polypyrrole thin film was synthesized by easy and economic chemical oxidative polymerization technique on glass at room temperature. The prepared thin film of Polypyrrole was characterized by optical absorbance study by UV-visible spectroscopy and electrical study by I-V measurement system. The optical absorbance spectrum of Polypyrrole shows two fundamental peaks in region of 420 and 890 nm, which confirms the formation of Polypyrrole on glass substrate. The I-V graph of nanostructured Polypyrrole represents the Ohmic nature. Furthermore, the thin film of Polypyrrole was investigated by Scanning electron microscopy for surface morphology study. The SEM micrograph represents spherical nanostructured morphology of Polypyrrole on glass substrate. In order to investigate gas sensing properties, 100 ppm of LPG, Ammonia and Nitrogen Dioxide were injected in the gas chamber and magnitude of resistance has been recorded as a function of time in second. It was observed that nanostructured Polypyrrole thin film shows good sensing behavior at room temperature.

  1. Electrical Transport Over Wide Temperature Range In Doped And Undoped Polypyrrole

    SciTech Connect

    Taunk, Manish; Chand, Subhash

    2010-12-01

    Polypyrrole was synthesized by chemical oxidation method by varying oxidant to monomer molar ratio for the optimization of electrical conductivity without using any external dopant. The conductivity in doped polypyrrole reached up to a maximum value of 7.2 S/cm. Neutralization of doped polypyrrole was done with aqueous ammonium hydroxide and three orders of reduced conductivity was obtained in neutral polypyrrole. Doping and neutralization of polypyrrole samples was supported by FTIR spectroscopy. Doped and undoped samples of polypyrrole were then electrically characterized over wide temperature range of 10-300 K. Stronger and weak temperature dependence of conductivity was revealed by undoped and doped polypyrrole samples respectively. An effort has been made to explore the electrical transport in doped and undoped polypyrrole by charge transport models. The experimental data obeys Kivelson's hopping model in temperature range of 60-300 K and fluctuation assisted tunneling was dominant conduction mechanism below 80 K.

  2. Use of a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin column and propionic acid as an eluent in ion-exclusion/adsorption chromatography of aliphatic carboxylic acids and ethanol in food samples.

    PubMed

    Mori, Masanobu; Hironaga, Takahiro; Kajiwara, Hiroe; Nakatani, Nobutake; Kozaki, Daisuke; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2011-01-01

    We developed an ion-exclusion/adsorption chromatography (IEAC) method employing a polystyrene-divinylbenzene-based weakly acidic cation-exchange resin (PS-WCX) column with propionic acid as the eluent for the simultaneous determination of multivalent aliphatic carboxylic acids and ethanol in food samples. The PS-WCX column well resolved mono-, di-, and trivalent carboxylic acids in the acidic eluent. Propionic acid as the eluent gave a higher signal-to-noise ratio, and enabled sensitive conductimetric detection of analyte acids. We found the optimal separation condition to be the combination of a PS-WCX column and 20-mM propionic acid. Practical applicability of the developed method was confirmed by using a short precolumn with a strongly acidic cation-exchange resin in the H(+)-form connected before the separation column; this was to remove cations from food samples by converting them to hydrogen ions. Consequently, common carboxylic acids and ethanol in beer, wine, and soy sauce were successfully separated by the developed method. PMID:21558657

  3. Polypyrrole hollow fiber for solid phase extraction.

    PubMed

    Tian, Tian; Deng, Jianjun; Xie, Zhuoying; Zhao, Yuanjin; Feng, Zhangqi; Kang, Xuejun; Gu, Zhongze

    2012-04-21

    We have developed a solid-phase extraction method based on conductive polypyrrole (PPy) hollow fibers which were fabricated by electrospinning and in situ polymerization. The electrospun poly (e-caprolactone) (PCL) fibers were employed as templates for the in situ surface polymerization of PPy under mechanical stirring or ultrasonication to obtain burr-shaped or smooth fiber shells, respectively. Hollow PPy fibers, achieved by removing the PCL templates, were the ideal sorbents for solid phase extraction of polar compounds due to their inherent multi-functionalities. By using the hollow PPy fibers, two important neuroendocrine markers of behavioural disorders, 5-hydroxyindole-3-acetic acid and homovanillic acid, were successfully extracted. Under the optimized conditions, the absolute recoveries of the above two neuroendocrine markers were 90.7% and 92.4%, respectively, in human plasma. Due to its simplicity, selectivity and sensitivity, the method may be applied to quantitatively analyse the concentrations of polar species in complex matrix samples. PMID:22398754

  4. Processing, Microstructure and Mechanical Behavior of Ultrasonic Assisted Cast Magnesium 1wt% Silicon Carbide Nano-Composites

    NASA Astrophysics Data System (ADS)

    Erman, Ari

    The goal of this dissertation is to establish an understanding of processing -- microstructure -- mechanical behavior relationship in Mg-1wt% SiC metal matrix nano-composites fabricated via an ultrasonic assisted casting process, with the emphasis on the effect of the distribution of nanoparticles on this relationship. Ultrasonic assisted casting has been proved as an effective technique to distribute nanoparticles in Mg metal matrix nano-composites (MMNCs). Mg MMNCs reinforced with 1 wt% SiC nanoparticles, were cast by ultrasonic cavitation-based dispersion methods. Microstructural analyses of as cast specimens were conducted to characterize the grain size, shape and distribution, SiC nanoparticle size and distribution, and nanoparticle-matrix interface. Average grain size for the ultrasonic assisted cast composite specimens was 72 mum compared to 181 mum for pure Mg samples prepared by the same method. The average measured SiC nanoparticle size was 66 nm. TEM studies showed good local dispersion of SiC nanoparticles, with only a few small, widely spaced clusters. HRTEM showed a clean interface between SiC nanoparticles and the Mg matrix, with no evidence of secondary phases. The yield strength of Mg-1 wt% SiC nanocomposites was 67 MPa, which showed improvement from 47 MPa for the pure Mg samples. This extra strengthening is due to Orowan and Hall-Petch effects. Fatigue experiments were conducted to characterize the cyclic stress-strain response of pure Mg and Mg-1wt% SiC samples at 0.2%, 0.4% and 0.6% plastic strain amplitudes. The analyses of the cyclic stress response curves and hysteresis loops, combined with post failure TEM analyses provided an understanding of the role of twinning, and twin-particle interactions on the cyclic deformation behavior of Mg MMNCs. Tensile twinning and basal slip are the main forms of deformation mechanisms under compression, followed by detwinning and basal slip in subsequent tension. Fatigue lives of Mg MMNCs are comparable to

  5. Direct electron transfer and sensing performance for catechin of nano-gold particles-polymer nano-composite with immobilized Laccase

    NASA Astrophysics Data System (ADS)

    Yang, Y.; Zeng, H.; Zhang, Q.; Bai, X.; Liu, C.; Zhang, Y. H.

    2016-08-01

    An electrochemical sensor for catechin detection was prepared. This sensor based on the electrode covered by nano-composite with Laccase. As-prepared nano-composite was made up of 4-mercaptobenzoic acid functionalized nano-gold particles and polymer. Site-directed adsorption of Lac in matrix led to stable immobilization of Lac and improved its direct electrochemistry. The Lac-based electrode was sensitive to catechin with high selectivity and low detection limit (16 nM). This novel sensor exhibited excellent reproducibility, long-term stability and high tolerance to enzyme inhibitor. Result of test in industrial sewage convinced the liability of Lac-based sensor characterized with high performance liquid chromatography and electrochemical method.

  6. Preparation of Nano-Composite Ca2-αZnα(OH)4 with High Thermal Storage Capacity and Improved Recovery of Stored Heat Energy

    NASA Astrophysics Data System (ADS)

    Zheng, M.; Sun, S. M.; Hu, J.; Zhao, Y.; Yu, L. J.

    2014-11-01

    Thermal energy storage has very important prospects in many applications related to the use of renewable energies (solar energy, etc.) or other energy sources, such as waste heat from industrial processes. Thermochemical storage is very attractive for long-term storage, since it could be conducted at room temperature without energy losses. In the present paper, a novel nanocomposite material, Ca2-αZnα(OH)4, is prepared using coprecipitation methodology and is characterized by XRD and DSC tests. The XRD result shows that the grain size of the nano-composite ranges from 40 nm to 95 nm. The DSC test result shows that the nano-composite exhibits high thermal storage capacity: 764.5 J/g at α = 0.8555. Its thermal decomposition temperature was found to be approximately 180º. Itwas found possible to recover 63.25% of the stored heat energy.

  7. Thermal decomposition assisted synthesis and upconversion property of Fe3O4@YPO4:Tm/Yb hybrid nano-composite phosphor

    NASA Astrophysics Data System (ADS)

    Tiwari, S. P.; Kumar, K.; Rai, V. K.

    2015-06-01

    Hybrid nano-composite phosphor has been successfully synthesized through thermal decomposition method. The dual phase of samples assigned by XRD analysis shows the formation of nano-composite with crystallite size 20 nm and 12 nm for YPO4: Tm/Yb and Fe3O4@YPO4:Tm/Yb respectively. The FESEM images show the spherical shape and non agglomerated formation of nanoparticles. Three bands in upconversion emission mode were found in intense blue at 472 nm, red at 662 nm and NIR at 798 nm regions corresponding to1G4 → 3H6, 1G4 → 3F4 and 3H4 → 3H6 transition states respectively. The lifetime for1G4 → 3H6 level is found 1150 microsecond and 1400 microsecond for YPO4: Tm/Yb and Fe3O4@YPO4:Tm/Yb samples respectively.

  8. Sulfur/graphitic hollow carbon sphere nano-composite as a cathode material for high-power lithium-sulfur battery

    NASA Astrophysics Data System (ADS)

    Shin, Eon Sung; Kim, Min-Seop; Cho, Won Il; Oh, Si Hyoung

    2013-08-01

    The intrinsic low conductivity of sulfur which leads to a low performance at a high current rate is one of the most limiting factors for the commercialization of lithium-sulfur battery. Here, we present an easy and convenient method to synthesize a mono-dispersed hollow carbon sphere with a thin graphitic wall which can be utilized as a support with a good electrical conductivity for the preparation of sulfur/carbon nano-composite cathode. The hollow carbon sphere was prepared from the pyrolysis of the homogenous mixture of the mono-dispersed spherical silica and Fe-phthalocyanine powder in elevated temperature. The composite cathode was manufactured by infiltrating sulfur melt into the inner side of the graphitic wall. The electrochemical cycling shows a capacity of 425 mAh g-1 at 3 C current rate which is more than five times larger than that for the sulfur/carbon black nano-composite prepared by simple ball milling.

  9. Multiscale simulation of polymer nano-composites (PNC) using molecular dynamics (MD) and generalized interpolation material point method (GIMP)

    NASA Astrophysics Data System (ADS)

    Nair, Abilash R.

    Recent mechanical characterization experiments with pultruded E-Glass / polypropylene (PP) and compression molded E-Glass/Nylon-6 composite samples with 3-4 weight% nanoclay and baseline polymer (polymer without nanoclay) confirmed significant improvements in compressive strength (˜122%) and shear strength (˜60%) in the nanoclay modified nanocomposites, in comparison with baseline properties. Uniaxial tensile tests showed a small increase in tensile strength (˜3.4%) with 3 wt % nanoclay loading. While the synergistic reinforcing influence of nanoparticle reinforcement is obvious, a simple rule-of-mixtures approach fails to quantify the dramatic increase in mechanical properties. Consequently, there is an immediate need to investigate and understand the mechanisms at the nanoscale that are responsible for such unprecedented strength enhancements. In this work, an innovative and effective method to model nano-structured components in a thermoplastic polymer matrix is proposed. Effort will be directed towards finding fundamental answers to the reasons for significant changes in mechanical properties of nanoparticle-reinforced thermoplastic composites. This research ensues a multiscale modeling approach in which (a) a concurrent simulations scheme is developed to visualize atomistic behavior of polymer molecules as a function of continuum scale loading conditions and (b) a novel nanoscale damage mechanics model is proposed to capture the constitutive behavior of polymer nano composites (PNC). The proposed research will contribute towards the understanding of advanced nanostructured composite materials, which should subsequently benefit the composites manufacturing industry.

  10. Fabrication of micro/nano-composite porous TiO2 electrodes for quantum dot-sensitized solar cells

    NASA Astrophysics Data System (ADS)

    Song, Xiaohui; Wang, Minqiang; Xing, Tiying; Deng, Jianping; Ding, Jijun; Yang, Zhi; Zhang, Xiangyu

    2014-05-01

    For colloidal quantum dots-sensitized solar cells (QDSSC), the penetration and distribution of quantum dots (QDs) within electrodes is very crucial for performance improvement. In view of much bigger size of colloidal QDs than that of dye molecules, a TiO2 electrode with open structure is helpful for the distribution of QDs. In this study, micro/nano-composite porous TiO2 electrodes are fabricated by incorporating polystyrene (PS) spheres into the TiO2 screen-printing paste. After sintering, the embedded PS spheres are burnt off, leaving randomly distributed submicrometer voids in the electrodes, which favor easy penetration of the colloidal CdSe QDs within the TiO2 electrodes, and thus avoiding the unfavorable clogging of pores by CdSe QDs. In addition, this kind of composite structure enhances the scattering properties of the electrodes and hence the light capture inside the device. In order to obtain optimized devices, we probe into the influence of the PS concentration on the photovoltaic performance. The result shows that a maximum conversion efficiency of 2.23% is obtained for the QDSSC made from the PS:TiO2 = 1:4 paste.

  11. Novel rare earth ions-doped oxyfluoride nano-composite with efficient upconversion white-light emission

    SciTech Connect

    Chen Daqin; Wang Yuansheng Yu Yunlong; Huang Ping; Weng Fangyi

    2008-10-15

    Transparent SiO{sub 2}-Al{sub 2}O{sub 3}-NaF-YF{sub 3} bulk nano-composites triply doped with Ho{sup 3+}, Tm{sup 3+} and Yb{sup 3+} were fabricated by melt-quenching and subsequent heating. X-ray diffraction and transmission electron microscopy measurements demonstrated the homogeneous precipitation of the {beta}-YF{sub 3} crystals with mean size of 20 nm among the glass matrix, and rare earth ions were found to partition into these nano-crystals. Under single 976 nm laser excitation, intense red, green and blue upconversion emissions were simultaneously observed owing to the successive energy transfer from Yb{sup 3+} to Ho{sup 3+} or Tm{sup 3+}. Various colors of luminescence, including bright perfect white light, can be easily tuned by adjusting the concentrations of the rare earth ions in the material. The overall energy efficiency of the white-light upconversion was estimated to be about 0.2%. - Graphical abstract: Under single 976 nm laser excitation, intense red, green and blue upconversion emissions were simultaneously observed owing to the successive energy transfer from Yb{sup 3+} to Ho{sup 3+} or Tm{sup 3+}. Various colors of luminescence, including bright perfect white light with CIE-X=0.351 and CIE-Y=0.306, can be easily tuned by adjusting the concentrations of the rare earth ions in the transparent oxyfluoride glass ceramics.

  12. Microstructural evolution and sliding wear studies of copper-alumina micro- and nano-composites fabricated by spark plasma sintering

    NASA Astrophysics Data System (ADS)

    Dash, Khushbu; Chaira, Debasis; Ray, Bankim Chandra

    2015-05-01

    Copper-alumina nanocomposites of 0.5, 1, 3, 5, 7 vol.% alumina (average size <50 nm) reinforced in copper matrix were fabricated using spark plasma sintering (SPS) technique. Another set of microcomposites containing 1, 5, 20 vol.% of alumina (average size ˜10 μm) had been fabricated to compare the physical as well as mechanical attributes of composites with variation of reinforcement particle size. These micro- and nano-composites have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), transmission electron microscopy (TEM) followed by microhardness, nanoindentation hardness, and wear measurements. It has been found that hardness values are higher for nanocomposites as compared to microcomposites. It is also found that wear resistance increases with increasing alumina content. The microcomposites show better wear resistance than nanocomposites for the same composition. The interaction of copper and alumina results in the formation of CuAlO2 which manifests differential interfacial phenomenon. We have obtained 95.82% densification and 93.17 HV hardness for spark plasma sintered Cu-20 vol.% Al2O3 microcomposite. The wear rate is appreciably low, that is, 0.86×10-4 mm3N-1m-1 for 20 vol.% alumina reinforced copper microcomposite.

  13. Nonlinear forced vibration response of smart two-phase nano-composite beams to external harmonic excitations

    NASA Astrophysics Data System (ADS)

    Mareishi, Soraya; Kalhori, Hamed; Rafiee, Mohammad; Hosseini, Seyedeh Marzieh

    2015-01-01

    This paper presents an analytical solution for nonlinear free and forced vibration response of smart laminated nano-composite beams resting on nonlinear elastic foundation and under external harmonic excitation. The structure is under a temperature change and an electric excitation through the piezoelectric layers. Different distribution patterns of the single walled aligned and straight carbon nanotubes (SWCNTs) through the thickness of the beam are considered. The beam complies with Euler-Bernoulli beam theory and von Kármán geometric nonlinearity. The nonlinearity is due to the mid-plane stretching of the beam and the nonlinear stiffness of the elastic foundation. The Multiple Time Scales perturbation scheme is used to perform the nonlinear dynamical analysis of functionally graded carbon nanotube-reinforced beams. Analytical expressions of the nonlinear natural frequencies, nonlinear dynamic response and frequency response of the system in the case of primary resonance have been presented. The effects of different parameters including applied voltage, temperature change, beam geometry, the volume fraction and distribution pattern of the carbon nanotubes on the nonlinear natural frequencies and frequency-response curves are presented. It is found that the volume fractions of SWCNTs as well as their distribution pattern significantly change the behavior of the system.

  14. A photoelectrochemical sensor based on CdS-polyamidoamine nano-composite film for cell capture and detection.

    PubMed

    Qian, Zheng; Bai, Hai-Jing; Wang, Guang-Li; Xu, Jing-Juan; Chen, Hong-Yuan

    2010-05-15

    We demonstrated herein a newly developed photoelectrochemical cell-sensor for the determination of SMMC-7721 human hepatoma carcinoma cells (SMMC-7721 cells) by using a photosensitive CdS-polyamidoamine (G4) nano-composite film (CdS-PAMAM). The film was generated by electrodeposition method. The presence of PAMAM in the film eliminated the surface defects of CdS nanoparticles and therefore resulted in a greatly enhanced photocurrent and a reduced dark current. In the presence of the electron donor ascorbic acid (AA), the photoexcitation of this modified electrode potentiostated at 0 V versus Ag/AgCl led to an anodic photocurrent. As a result of the covalent coupling reactions, a layer of concanavalin A (ConA) was firmly bound to the functionalized CdS-PAMAM film via glutaraldehyde bridges. The resulting modified electrodes were tested as sensors for SMMC-7721 cell capture and detection via affinity interactions between ConA and mannosyl groups on cell surface. The cell concentration was measured from 5.0 x 10(3) to 1.0 x 10(7) cells mL(-1) through the decrease in photocurrent intensity resulting from its specific binding onto the photosensitive film, the detection limit being 5.0 x 10(3) cells mL(-1). PMID:20181470

  15. Synthesis and biological response of casein-based silica nano-composite film for drug delivery system.

    PubMed

    Ma, Jianzhong; Xu, Qunna; Zhou, Jianhua; Zhang, Jing; Zhang, Limin; Tang, Huiru; Chen, Lihong

    2013-11-01

    Casein possesses many interesting properties that make it a good candidate for conventional and novel drug delivery systems. In this study, casein-based silica nano-composite was prepared via double in situ method, and the as-prepared latex particles were evaluated in terms of their morphology and size through transmission electron microscopy (TEM). The film morphology was investigated by scanning electron microscopy (SEM) and energy dispersive X-ray (EDX), and the mechanical property and response behavior of the films as a function of silica content were discussed. Ibuprofen was used as the model drug. The drug load and release properties were studied by solid-state nuclear magnetic resonance (solid-state NMR), Fourier transform infrared (FT-IR), SEM and in vitro test. The composite latex particle showed a stable core-shell structure, and the film exhibited a regular surface with even SiO2 distribution. The drug load efficiency of the composite films increased with adding silica because of the adsorption of the drugs on the silica. In an acidic release medium, the ibuprofen-loaded composite showed a slower drug release dependent on the silica content. These behaviors were most likely due to the reduced diffusion rate of the drug through the composite microsphere, which resulted from the interaction between the silica and the drug. PMID:23831671

  16. Evaluation of separation properties of a modified strong cation exchange material named MEX and its application in 2D-MEX × C18 system to separate peptides from scorpion venom.

    PubMed

    Chen, Bo; Xu, Junyan; Fu, Qing; Dong, Xuefang; Guo, Zhimou; Jin, Yu; Liang, Xinmiao

    2015-07-01

    Peptides from scorpion venom represent one of the most promising drug sources for drug discovery for some specific diseases. Current challenges in their separation include high complexity, high homologies and the huge range of peptides. In this paper, a modified strong cation exchange material, named MEX, was utilised for the two-dimensional separation of peptides from complex scorpion venom. The silica-based MEX column was bonded with two functional groups; benzenesulfonic acid and cyanopropyl. To better understand its separation mechanisms, seven standard peptides with different properties were employed in an evaluation study, the results of which showed that two interactions were involved in the MEX column: electrostatic interactions based on benzenesulfonic acid groups dominated the separation of peptides; weak hydrophobic interactions introduced by cyanopropyl groups increased the column's selectivity for peptides with the same charge. This characteristic allowed the MEX column to overcome some of the drawbacks of traditional strong cation exchange (SCX) columns. Furthermore, the study showed the great effects of the acetonitrile (ACN) content, the sodium perchlorate (NaClO4) concentration and the buffer pH in the mobile phase on the peptides' retention and separation selectivity on the MEX column. Subsequently, the MEX column was combined with a C18 column to establish an off-line 2D-MEX × C18 system to separate peptides from scorpion Buthus martensi Karsch (BmK) venom. Due to complementary separation mechanisms in each dimension, a high orthogonality of 47.62% was achieved. Moreover, a good loading capacity, excellent stability and repeatability were exhibited by the MEX column, which are beneficial for its use in future preparation experiments. Therefore, the MEX column could be an alternative to the traditional SCX columns for the separation of peptides from scorpion venom. PMID:25996445

  17. Detachable strong cation exchange monolith, integrated with capillary zone electrophoresis and coupled with pH gradient elution, produces improved sensitivity and numbers of peptide identifications during bottom-up analysis of complex proteomes.

    PubMed

    Zhang, Zhenbin; Yan, Xiaojing; Sun, Liangliang; Zhu, Guijie; Dovichi, Norman J

    2015-04-21

    A detachable sulfonate-silica hybrid strong cation-exchange monolith was synthesized in a fused silica capillary, and used for solid phase extraction with online pH gradient elution during capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) proteomic analysis. Tryptic digests were prepared in 50 mM formic acid and loaded onto the strong cation-exchange monolith. Fractions were eluted using a series of buffers with lower concentration but higher pH values than the 50 mM formic acid background electrolyte. This combination of elution and background electrolytes results in both sample stacking and formation of a dynamic pH junction and allows use of relatively large elution buffer volumes while maintaining reasonable peak efficiency and resolution. A series of five pH bumps were applied to elute E. coli tryptic peptides from the monolith, followed by analysis using CZE coupled to an LTQ-Orbitrap Velos mass spectrometer; 799 protein groups and 3381 peptides were identified from 50 ng of the digest in a 2.5 h analysis, which approaches the identification rate for this organism that was obtained with an Orbitrap Fusion. We attribute the improved numbers of peptide and protein identifications to the efficient fractionation by the online pH gradient elution, which decreased the complexity of the sample in each elution step and improved the signal intensity of low abundance peptides. We also performed a comparative analysis using a nanoACQUITY UltraPerformance LCH system. Similar numbers of protein and peptide identifications were produced by the two methods. Protein identifications showed significant overlap between the two methods, whereas peptide identifications were complementary. PMID:25822566

  18. Polypyrrole-Based Implantable Electroactive Pump for Controlled Drug Microinjection.

    PubMed

    Yan, Bingxi; Li, Boyi; Kunecke, Forest; Gu, Zhen; Guo, Liang

    2015-07-15

    Implantable devices for long-lasting controlled insulin microinjection are of great value to diabetic patients. To address this need, we develop a flexible electroactive pump based on a biocompatible polypyrrole composite film that comprises a polypyrrole matrix and a macromolecular dopant of polycaprolactone-block-polytetrahydrofuran-block-polycaprolactone. Using phosphate-buffered saline as the electrolyte, this film demonstrates much higher electroactivity and reproducibility than conventional Cl--doped polypyrrole, making it an excellent actuator for driving an implantable pump. At a driving current density of 1 mA/cm2, the pump demonstrates a consistent output capacity of 10.5 at 0.35 μL/s over 20 cycles. This work paves the way for the development of an implantable electroactive pump to improve the quality of life of diabetics. PMID:26134590

  19. Highly sensitive DNA sensor based on polypyrrole nanowire

    NASA Astrophysics Data System (ADS)

    Mai, Anh Tuan; Duc, Thanh Pham; Thi, Xuan Chu; Nguyen, Minh Hieu; Nguyen, Hoang Hai

    2014-08-01

    This paper describes the development of a DNA sensor based on polypyrrole nanowire. By using potentiostatic technique, in the presence of gelatin as the soft mold, the polypyrrole nanowires were synthesized on the surface of the micro-sensor. The surface enhanced Raman spectroscopy shows that the Nsbnd H ends of the polypyrrole nanowires orientate upward from the surface facilitating the DNA probe immobilization through the simple linkage with the phosphate groups of the probe DNA. The label-free signal readout was carried out by lock-in amplifier technique. The response time of the DNA sensor is 10 s and the measurement time was 5 min. The lowest detectable concentration of Escherichia coli DNA was 0.1 nM.

  20. Structural and electrical characterization of hybrid metal-polypyrrole nanowires

    NASA Astrophysics Data System (ADS)

    Gence, L.; Faniel, S.; Gustin, C.; Melinte, S.; Bayot, V.; Callegari, V.; Reynes, O.; Demoustier-Champagne, S.

    2007-09-01

    We present here the synthesis and structural characterization of hybrid Au-polypyrrole-Au and Pt-polypyrrole-Au nanowires together with a study of their electrical properties from room temperature down to very low temperature. A careful characterization of the metal-polymer interfaces by transmission electron microscopy revealed that the structure and mechanical strength of bottom and upper interfaces are very different. Variable temperature electrical transport measurements were performed on both multiple nanowires—contained within the polycarbonate template—and single nanowires. Our data show that the three-dimensional Mott variable-range-hopping model provides a complete framework for the understanding of transport in polypyrrole nanowires, including nonlinear current-voltage characteristics and magnetotransport at low temperatures.

  1. Non-aqueous polypyrrole colloids: Synthesis and characterization

    SciTech Connect

    Armes, S.P.; Aldissi, Mahmoud

    1989-01-01

    The preparation of sterically-stabilized polypyrrole colloids via a dispersion polymerization route in non-aqueous media is described for the first time. Pyrrole polymerization was achieved using FeCl/sub 3/ as an oxidant/dopant in organic solvents such as methyl acetate, methyl formate and propyl formate. Macroscopic precipitation was prevented by the use of poly (vinyl acetate) as a polymeric surfactant. Other surfactants, used successfully in aqueous media, were incompatible and consequently resulted in precipitation of polypyrrole. Several techniques were used for characterization of the dispersions including transmission and scanning electron microscopies (TEM and SEM), thermogravimetric analysis (TGA), velocity charge analysis and visible absorption spectroscopy. TEM indicated a polydisperse spherical morphology with a particle diameter in the range 100-300 nm. The compressed pellet conductivity of the dried dispersion was 0.1 S/cm. These dispersions are often compared with aqueous bulk polypyrrole and aqueous dispersions. 11 refs., 3 figs., 1 tab.

  2. Influence of Hydroxyapatite Nano-particles on the Mechanical and Tribological Properties of Orthopedic Cement-Based Nano-composites Measured by Nano-indentation and Nano-scratch Experiments

    NASA Astrophysics Data System (ADS)

    Asgharzadeh Shirazi, H.; Ayatollahi, M. R.; Naimi-Jamal, M. R.

    2015-09-01

    The aim of this study was to examine the mechanical and tribological properties of a commercially available bone cement by incorporating nano-sized hydroxyapatite using nano-indentation and nano-scratch experiments. In order to achieve this goal, the nano-composite cement samples with different amounts of commercial nano-hydroxyapatite (HAc), as a bone compatible nano-filler, were prepared via vacuum mixing method. The results indicated that nano-indentation and nano-scratch experiments are acceptable methods for measuring the mechanical and tribological properties of orthopedic cement-based nano-composites. Moreover, it was found that the nano-composite of 10 wt.% HAc exhibits the optimum performance compared to the other nano-composite samples in terms of mechanical and tribological properties. These findings can play an important role in achieving the goal of clinical and biomechanical function optimization of bone cement, especially in the field of orthopedic surgery.

  3. Magnetization enhancement due to incorporation of non-magnetic nitrogen content in (Co84Zr16)Nx nano-composite films

    NASA Astrophysics Data System (ADS)

    Singh, Jitendra; Shukla, Rishabh; Bagri, Anita; Dhaka, Rajendra S.; Akhtar, Jamil

    2016-01-01

    We report the magnetic, electronic, and structural properties of nano-composite (Co84Zr16)Nx or CZN films prepared by reactive co-sputter deposition method. As-deposited CZN films have shown enhancement in magnetization (Ms) with incorporation of nitrogen content, which is related to the evolution of nano-composite phase. X-ray diffraction study has confirmed poly-crystalline growth of CZN films with fcc(331) and fcc(422) phases. High-resolution transmission electron microscope study reveals that CZN films are composed of ordered and crystalline ferromagnetic Co nano-clusters, which are embedded in the nano-composite matrix. Photoemission measurements show the change in the intensity near the Fermi level most likely due to defects and shift in the core-levels binding energy with nitrogen concentration. Raman spectroscopy data show an increase in the intensity of the Raman lines with nitrogen concentration upto 20%. However, the intensity is significantly lower for 30% sample. This indicates that less nitrogen or defect states are being substituted into the lattice above 20% and is consistent with the observed magnetic behavior. Our studies indicate that defects induced due to the incorporation of non-magnetic nitrogen content play a key role to enhance the magnetization.

  4. Effect of nano-composite and Thyme oil (Tymus Vulgaris L) coating on fruit quality of sweet cherry (Takdaneh Cv) during storage period.

    PubMed

    Nabifarkhani, Naser; Sharifani, Mehdi; Daraei Garmakhany, Amir; Ganji Moghadam, Ebrahim; Shakeri, Alireza

    2015-07-01

    Sweet cherry is one of the most appreciated fruit by consumers since it is an early season fruit and has an excellent quality. In this study effect of active nano composite formed from chitosan (as a matrix material), nano cellulose fiber (1% concentration) and Thyme oils (Tymus Vulgaris L) at 1% concentration on fruits quality was investigated. Treated fruits were stored at 1°C for 5 weeks and changes of different qualities attributes including weight loss, total acidity, TSS, anthocyanin, total sugar and malic acid content (by high performance liquid chromatography (HPLC) method) were measured each week. Results showed that nano composite and Thyme oil significantly affect fruit's water retention and so decrease fruit weight loss and preserve anthocyanin (P < 0.05). None of applied treatments had any significant effects in comparison with control in regard to acidity while total sugar content and TSS significantly affected by treatment compared to control samples. Result of HPLC analysis showed that there was no significant difference between different treatment and control sample in term of malic acid concentrations during storage period but increase storage time lead to increase malic acid concentration in all treatments. For conclusion it can be Saied that fruits coating with nano-composite, lead to increase fruit shelf life, better appearance and prevents fungal growth that may be due to creation of an active packaging by these compounds. PMID:26288725

  5. Effect of nano-composite and Thyme oil (Tymus Vulgaris L) coating on fruit quality of sweet cherry (Takdaneh Cv) during storage period

    PubMed Central

    Nabifarkhani, Naser; Sharifani, Mehdi; Daraei Garmakhany, Amir; Ganji Moghadam, Ebrahim; Shakeri, Alireza

    2015-01-01

    Sweet cherry is one of the most appreciated fruit by consumers since it is an early season fruit and has an excellent quality. In this study effect of active nano composite formed from chitosan (as a matrix material), nano cellulose fiber (1% concentration) and Thyme oils (Tymus Vulgaris L) at 1% concentration on fruits quality was investigated. Treated fruits were stored at 1°C for 5 weeks and changes of different qualities attributes including weight loss, total acidity, TSS, anthocyanin, total sugar and malic acid content (by high performance liquid chromatography (HPLC) method) were measured each week. Results showed that nano composite and Thyme oil significantly affect fruit's water retention and so decrease fruit weight loss and preserve anthocyanin (P < 0.05). None of applied treatments had any significant effects in comparison with control in regard to acidity while total sugar content and TSS significantly affected by treatment compared to control samples. Result of HPLC analysis showed that there was no significant difference between different treatment and control sample in term of malic acid concentrations during storage period but increase storage time lead to increase malic acid concentration in all treatments. For conclusion it can be Saied that fruits coating with nano-composite, lead to increase fruit shelf life, better appearance and prevents fungal growth that may be due to creation of an active packaging by these compounds. PMID:26288725

  6. Mathematical model of a lithium/polypyrrole cell

    NASA Technical Reports Server (NTRS)

    Yeu, Taewhan; White, Ralph E.

    1990-01-01

    A mathematical model to simulate the charge/discharge behavior of a lithium/lithium perchlorate-propylene carbonate/polypyrrole secondary battery cell is presented. The model can be used to gain a better understanding of the behavior of this cell and to provide guidance toward the design of new secondary batteries which utilize an electronically conductive polymer such as polypyrrole as the cathode. The model includes the capability of handling charge and discharge behavior and is used to study the effect of various design parameters on the performance of the cell.

  7. Conductive polypyrrole/viscose fiber composites.

    PubMed

    Wang, Ning; Li, Guodong; Yu, Zhuo; Zhang, Xingxiang; Qi, Xiaoling

    2015-08-20

    Polypyrrole (PPy) was polymerized with pyrrole (Py) as the monomer, FeCl3 as an oxidant and sodium dodecyl benzene sulfonate (SDBS) as the dopant on the surface of viscose fiber (VCF) to prepare the conductive PPy/VCF composites. Fourier transform infrared spectra (FT-IR), thermal gravimetric analysis (TGA) and X-ray photoelectron spectroscope (XPS) proved that the interaction between PPy and VCF formed in the PPy/VCF composites. Three structures of N atoms (imine, amine and cationic atoms) were found in PPy of PPy/VCF composites. The influence of reaction conditions including reaction time, Py concentration, FeCl3 concentration and SDBS concentration on the morphology and the conductivity of PPy/VCF composites was investigated in detail. The orthogonal experiments were designed to determine the optimal reaction conditions: reaction time 5h, Py concentration 0.1 mol/L and FeCl3 concentration 0.25 mol/L. When PPy/VCF composite was washed 50 times in water, the conductivity still kept at 1.5S/cm, and this value was stable for more washing. PMID:25965491

  8. Polypyrrole nanostructures and their field emission investigations

    NASA Astrophysics Data System (ADS)

    Harpale, Kashmira; More, Mahendra A.; Koinkar, Pankaj M.; Patil, Sandip S.; Sonawane, Kishor M.

    2015-03-01

    Polypyrrole (PPy) nanostructures have been synthesized on indium doped tin oxide (ITO) substrates by a facile electrochemical route employing cyclic voltammetry (CV) mode. The morphology of the PPy thin films was observed to be influenced by the monomer concentration. Furthermore, FTIR revealed formation of electrically conducting state of PPy. Field emission investigations of the PPy nanostructures were carried out at base pressure of 1×10-8mbar. The values of turn-on field, corresponding to emission current density of 1 μA/cm2 were observed to be 0.6, 1.0 and 1.2 V/μm for the PPy films characterized with rod-like, cauliflower and granular morphology, respectively. In case of PPy nanorods maximum current density of 1.2 mA/cm2 has been drawn at electric field of 1 V/μm. The low turn on field, extraction of very high emission current density at relatively lower applied field and good emission stability propose the PPy nanorods as a promising material for field emission based devices.

  9. Size Dependent Antioxidant Activity of Polypyrrole Nanofibers

    NASA Astrophysics Data System (ADS)

    Kumar, A.; Banerjee, Somik

    2011-07-01

    Polypyrrole (PPy) nanofibers have been synthesized employing surfactant assisted miceller polymerization by varying the surfactant concentration. The synthesized nanofibers have been characterized using TEM, XRD, FTIR and UV-Visible spectroscopy. TEM reveals that the diameter of the PPy nanowires decreases with the increase in surfactant concentration. X-ray spectra shows an amorphous peak centered around 2θ = 24.6° which is attributed to the π-π interaction of the partial PPy chains similar to that of aromatic groups. The domain length of the samples determined using the single-line approximation technique, decreases with decreasing diameter whereas the strain in the material increases, which have been attributed to the reduction of size with increase in the surfactant concentration as revealed by TEM. The vibrational bands observed from the FTIR spectra confirm the formation of surfactant free PPy nanowires. UV-Visible spectra shows a blue-shift in the π-π* absorption peak. Antioxidant activity of the samples has been determined using the DPPH free radical method. It has been observed that enhancement in free radical scavenging coincides with the decreasing diameter of the PPy nanofibers which has been associated with the increase in the surface reaction sites with the reduction of size.

  10. An in vivo evaluation of PLLA/PLLA-gHA nano-composite for internal fixation of mandibular bone fractures.

    PubMed

    Peng, Weihai; Zheng, Wei; Shi, Kai; Wang, Wangshu; Shao, Ying; Zhang, Duo

    2015-12-01

    Internal fixation of bone fractures using biodegradable poly(L-lactic-acid) (PLLA)-based materials has attracted the attention of many researchers. In the present study, 36 male beagle dogs were randomly assigned to two groups: PLLA/PLLA-gHA (PLLA-grafted hydroxyapatite) group and PLLA group. PLLA/PLLA-gHA and PLLA plates were embedded in the muscular bags of the erector spinae and also implanted to fix mandibular bone fractures in respective groups. At 1, 2, 3, 6, 9, and 12 months postoperatively, the PLLA/PLLA-gHA and PLLA plates were evaluated by adsorption and degradation tests, and the mandibles were examined through radiographic analysis, biomechanical testing, and histological analysis. The PLLA/PLLA-gHA plates were non-transparent and showed a creamy white color, and the PLLA plates were transparent and faint yellow in color. At all time points following surgery, adsorption and degradation of the PLLA/PLLA-gHA plates were significantly less than those of the PLLA plates, and the lateral and longitudinal bending strengths of the surgically treated mandibles of the beagle dogs in the PLLA/PLLA-gHA group were significantly greater than those of the PLLA group and reached almost the value of intact mandibles at 12 months postoperatively. Additionally, relatively rapid bone healing was observed in the PLLA/PLLA-gHA group with the formation of new lamellar bone tissues at 12 months after the surgery. The PLLA/PLLA-gHA nano-composite can be employed as a biodegradable material for internal fixation of mandibular bone fractures. PMID:26551378

  11. Ti-TiC-TiC/DLC gradient nano-composite film on a biomedical NiTi alloy.

    PubMed

    Zheng, Yufeng; Liu, Dong; Liu, Xiliang; Li, Li

    2008-12-01

    Ti-TiC-TiC/diamond-like carbon (DLC) gradient nano-composite films have been prepared on NiTi alloy substrates by the technique of plasma immersion ion implantation and deposition (PIIID) combined with plasma-enhanced chemical vapor deposition (PECVD). The influence of negative bias voltage applied to the substrate (from -100 V to -500 V) on the chemical structure, microstructure, mechanical properties and corrosion resistance was investigated by Raman spectrum, x-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), x-ray diffraction (XRD), friction coefficient test, scratch test, nano-indentation test and anodic polarization experiments. The Raman spectrum and XPS results showed that the doped films kept an amorphous DLC structure. TEM observation revealed that nanometer TiC particles were surrounded by the amorphous DLC. With the increase of bias voltage, the ratio of sp(2)/sp(3) first decreased, reaching a minimum value at -200 V, and then increased. The nano-indentation results showed that the hardness of the Ti-TiC-TiC/DLC gradient films reached the maximum value at -200 V when TiC particles reached the maximum content in the films. The friction coefficient test and scratch test indicated that Ti-TiC-TiC/DLC gradient films had a low friction coefficient and high bonding strength with the NiTi substrates. Combined with anodic polarization curves and SEM observation, it was found that the corrosion resistance of the Ti-TiC-TiC/DLC gradient films was much better than that of the bare NiTi alloy. PMID:19029600

  12. Multifunctional, Highly Flexible, Free-Standing 3D Polypyrrole Foam.

    PubMed

    Wang, Chunhui; Ding, Yujie; Yuan, Ye; Cao, Anyuan; He, Xiaodong; Peng, Qingyu; Li, Yibin

    2016-08-01

    Multifunctional, highly flexible 3D polypyrrole (PPy) foam is fabricated via a simple electrodeposition method by using nickel foam as the template. The 3D PPy foam has a unique interior structure and is robust enough to manipulate directly. PMID:27357260

  13. ROOM TEMPERATURE BULK SYNTHESIS OF SILVER NANOCABLES WRAPPED WITH POLYPYRROLE

    EPA Science Inventory

    Wet chemical synthesis of silver cables wrapped with polypyrrole is reported in aqueous media without use of any surfactant/capping agent and/or template. The method employs direct polymerization of pyrrole of an aqueous solution with AgNO3 as an oxidizing agent. The four probe c...

  14. The application of a polypyrrole precoat for the metallization of printed circuit boards

    SciTech Connect

    Gottesfeld, S.; Uribe, F.A.; Armes, P. )

    1992-01-01

    This paper describes a printed circuit board metallization process starting with the formation of a percent of polypyrrole (PPY) on the board, followed by the direct electrodeposition of copper onto the polypyrrole-coated substrate. The polypyrrole film is applied to the insulating substrate by a single chemical polymerization step from an aqueous solution. The sheet resistance of the polypyrrole precoat is typically of the order of a few hundred {Omega}/{open square} which is a sufficiently low resistance to enable direct metal electrodeposition onto the PPY-coated substrate.

  15. Synthesis, characterisation and methyl orange adsorption capacity of ferric oxide-biochar nano-composites derived from pulp and paper sludge

    NASA Astrophysics Data System (ADS)

    Chaukura, Nhamo; Murimba, Edna C.; Gwenzi, Willis

    2016-02-01

    A Fe2O3-biochar nano-composite (Fe2O3-BC) was prepared from FeCl3-impregnated pulp and paper sludge (PPS) by pyrolysis at 750 °C. The characteristics and methyl orange (MO) adsorption capacity of Fe2O3-BC were compared to that of unactivated biochar (BC). X-ray diffraction (XRD) and scanning electron microscopy (SEM) confirmed the composite material was nano-sized. Fourier transform infrared (FTIR) spectroscopy revealed the presence of hydroxyl and aromatic groups on BC and on Fe2O3-BC, but Brunauer-Emmett-Teller (BET) surface area and Barrett-Joyner-Halenda (BJH) porosity were lower for Fe2O3-BC than BC. Despite the lower BET surface area and porosity of Fe2O3-BC, its MO adsorption capacity was 52.79 % higher than that of BC. The equilibrium adsorption data were best represented by the Freundlich model with a maximum adsorption capacity of 20.53 mg g-1 at pH 8 and 30 min contact time. MO adsorption obeyed pseudo-second-order kinetics for both BC and Fe2O3-BC with R 2 values of 0.996 and 0.999, respectively. Higher MO adsorption capacity for Fe2O3-BC was attributed to the hybrid nature of the nano-composites; adsorption occurred on both biochar matrix and Fe2O3 nanocrystals. Gibbs free energy calculations confirmed the adsorption is energetically favourable and spontaneous with a high preference for adsorption on both adsorbents. The nano-composite can be used for the efficient removal of MO (>97 %) from contaminated wastewater.

  16. A combined powder melt and infiltration growth technique for fabricating nano-composited Y-Ba-Cu-O single-grain superconductor

    NASA Astrophysics Data System (ADS)

    Li, Guo-Zheng; Li, Jia-Wei; Yang, Wan-Min

    2015-10-01

    The top-seeded melt growth (MG) and infiltration growth (IG) techniques are the two most popular methods of fabricating single-grain Y-Ba-Cu-O (YBCO) bulk superconductors, which are also considered as two distinctly different processes. In this study, we report a combined powder melt and infiltration growth (PM-IG) technique for fabricating nano-composited YBCO single-grain superconductors using raw metallic oxides. In this new technique, a solid source pellet (SSP) of composition nano-Y2O3 + BaO + CuO + 1 wt.%CeO2 and a liquid source pellet (LSP) of composition nano-Y2O3 + 10BaO + 16CuO are employed, thus during heat treatment process the powder melt in SSP (corresponding to the final YBCO bulk) and liquid infiltration from LSP to SSP coexist. Because the process of precursor powder synthesis is avoided, the fabrication flow is much simplified and the experimental efficiency is increased significantly. Microstructural observation indicates that a large number of Y2BaCuO5 nano-inclusions (around 100 nm) are trapped in the YBa2Cu3O7-δ superconducting matrix. Measurements of levitation force and trapped field prove the superior performance of the nano-composited YBCO sample. The calculated zero-field J c at 77 K reaches 6.98 × 104 A cm-2, nearly 23% higher than the sample fabricated by the conventional IG technique. Thus, this study supplies a practical method for fabricating nano-composited YBCO bulk superconductors with high performance.

  17. Y2O3-MgO Nano-Composite Synthesized by Plasma Spraying and Thermal Decomposition of Solution Precursors

    NASA Astrophysics Data System (ADS)

    Muoto, Chigozie Kenechukwu

    This research aims to identify the key feedstock characteristics and processing conditions to produce Y2O3-MgO composite coatings with high density and hardness using solution precursor plasma spray (SPPS) and suspension plasma spray (SPS) processes, and also, to explore the phenomena involved in the production of homogenized nano-composite powders of this material system by thermal decomposition of solution precursor mixtures. The material system would find potential application in the fabrication of components for optical applications such as transparent windows. It was shown that a lack of major endothermic events during precursor decomposition and the resultant formation of highly dense particles upon pyrolysis are critical precursor characteristics for the deposition of dense and hard Y2O3-MgO coatings by SPPS. Using these principles, a new Y2O3-MgO precursor solution was developed, which yielded a coating with Vickers hardness of 560 Hv. This was a considerable improvement over the hardness of the coatings obtained using conventional solution precursors, which was as low as 110 Hv. In the thermal decomposition synthesis process, binary solution precursor mixtures of: yttrium nitrate (Y[n]) or yttrium acetate (Y[a]), with magnesium nitrate (Mg[n]) or magnesium acetate (Mg[a]) were used in order to study the effects of precursor chemistry on the structural characteristics of the resultant Y2O3-MgO powders. The phase domains were coarse and distributed rather inhomogeneously in the materials obtained from the Y[n]Mg[n] and Y[a]Mg[a] mixtures; finer and more homogeneously-distributed phase domains were obtained for ceramics produced from the Y[a]Mg[n] and Y[n]Mg[a] mixtures. It was established that these phenomena were related to the thermal characteristics for the decomposition of the precursors and their effect on phase separation during oxide crystallization. Addition of ammonium acetate to the Y[n[Mg[n] mixture changed the endothermic process to exothermic

  18. Biocompatibility Implications of Polypyrrole Synthesis Techniques

    PubMed Central

    Fonner, John M.; Forciniti, Leandro; Nguyen, Hieu; Byrne, James; Kou, Yann-Fuu; Syeda-Nawaz, Jeja; Schmidt, Christine E.

    2008-01-01

    Polypyrrole (PPy) is an inherently conducting polymer that has shown great promise for biomedical applications within the nervous system. However, to effectively use PPy as a biomaterial implant, it is important to understand and reproducibly control the electrical properties, physical topography, and surface chemistry of the polymer. Although there is much research published on the use of PPy in various applications, there is no systematic study linking the methodologies used for PPy synthesis to PPy’s basic polymeric properties (e.g., hydrophilicity, surface roughness), and to the biological effects these properties have on cells. Electrochemically synthesized PPy films differ greatly in their characteristics depending on synthesis parameters such as dopant, substrate, and thickness, among other parameters. In these studies, we have used three dopants (chloride (Cl), tosylate (ToS), polystyrene sulfonate (PSS)), two substrates (gold and indium tin oxide-coated glass), and a range of thicknesses, to measure and compare the biomedically-important characteristics of surface roughness, contact angle, conductivity, dopant stability, and cell adhesion (using PC-12 cells and Schwann cells). As predicted, we discovered large differences in roughness depending on the dopant used and the thickness of the film, while substrate choice had little effect. From contact angle measurements, PSS was found to yield the most hydrophilic material, most likely because of free charges from the long PSS chains exposed on the surface of the PPy. ToS-doped PPy films were tenfold more conductive than Cl- or PSS-doped films. X-ray photoelectron spectroscopy studies were used to evaluate dopant concentrations of PPy films stored in water and phosphate buffered saline over 14 days, and conductance studies over the same timeframe measured electrical stability. PSS proved to be the most stable dopant, though all films experienced significant decay in conductivity and dopant concentration

  19. Application of enzymes, sodium tripolyphosphate and cation exchange resin for the release of extracellular polymeric substances from sewage sludge. Characterization of the extracted polysaccharides/glycoconjugates by a panel of lectins.

    PubMed

    Wawrzynczyk, J; Szewczyk, E; Norrlöw, O; Dey, E Szwajcer

    2007-06-30

    The study describes extraction of extracellular polymeric substances (EPS) from sewage sludge by applying enzymes and enzymes combined with sodium tripolyphosphate (STPP). Additionally, a systematic study of two non-enzymatic extraction agents is described. The assessment of the released products is made by colorimetrical methods and polysaccharides/glycoconjugates identification by the interaction with four immobilized lectins. Bio-sludge from Helsingborg (Sweden) and Damhusåen (Denmark) were used as two case studies for testing enzymatic extractability and thereby to make useful prediction of sludge bio-digestibility. From Helsingborg sludge the enzymes extracted about 40% more of EPS than from Damhusåen. The polysaccharides/glycoconjugates in both sludges maintained the same level, and showed substantial different interaction motifs with lectins panel. Damhusåen enzymatic extracted EPS had an enhanced amount of suspended material that was post-hydrolysed by the use of polygalacturonase and lysozyme resulting in pectin like polymers and petiptidoglycans. Petiptidoglycan is a marker from bacterial cell debris. STPP and cation exchange resin (CER) released different quantities of EPS. The CER released polysaccharides/glycoconjugates had higher molecular weight and stronger affinity towards Concanavalin A than the one released by the action of STPP. Independent of the extraction conditions, STPP released elevated amounts of polyvalent cations and humic substances in contrast to the very low amounts of released by CER. PMID:17543410

  20. Fully automated multidimensional reversed-phase liquid chromatography with tandem anion/cation exchange columns for simultaneous global endogenous tyrosine nitration detection, integral membrane protein characterization, and quantitative proteomics mapping in cerebral infarcts.

    PubMed

    Quan, Quan; Szeto, Samuel S W; Law, Henry C H; Zhang, Zaijun; Wang, Yuqiang; Chu, Ivan K

    2015-10-01

    Protein tyrosine nitration (PTN) is a signature hallmark of radical-induced nitrative stress in a wide range of pathophysiological conditions, with naturally occurring abundances at substoichiometric levels. In this present study, a fully automated four-dimensional platform, consisting of high-/low-pH reversed-phase dimensions with two additional complementary, strong anion (SAX) and cation exchange (SCX), chromatographic separation stages inserted in tandem, was implemented for the simultaneous mapping of endogenous nitrated tyrosine-containing peptides within the global proteomic context of a Macaca fascicularis cerebral ischemic stroke model. This integrated RP-SA(C)X-RP platform was initially benchmarked through proteomic analyses of Saccharomyces cerevisiae, revealing extended proteome and protein coverage. A total of 27 144 unique peptides from 3684 nonredundant proteins [1% global false discovery rate (FDR)] were identified from M. fascicularis cerebral cortex tissue. The inclusion of the S(A/C)X columns contributed to the increased detection of acidic, hydrophilic, and hydrophobic peptide populations; these separation features enabled the concomitant identification of 127 endogenous nitrated peptides and 137 transmembrane domain-containing peptides corresponding to integral membrane proteins, without the need for specific targeted enrichment strategies. The enhanced diversity of the peptide inventory obtained from the RP-SA(C)X-RP platform also improved analytical confidence in isobaric tags for relative and absolute quantitation (iTRAQ)-based proteomic analyses. PMID:26335518

  1. Flexibility of the zeolite RHO framework. In situ X-ray and neutron powder structural characterization of cation-exchanged BePO and BeAsORHO analogs

    SciTech Connect

    Nenoff, T.M.; Parise, J.B.; Jones, G.A.; Galya, L.G.; Corbin, D.R.; Stucky, G.D.

    1996-08-15

    This is an extensive study of the non-aluminosilicate analogs of the zeolite RHO. This molecular sieve is of great interest commercially because of its catalytic properties. In the absence of rigid supporting structural subunits (smaller cages or channels), the aluminosilicate RHO exhibits atypical framework flexibility with large displacivere arrangements. The beryllophosphate and beryalloarsenate analogs are easily synthesized under very mild reaction conditions and therefore maybe of interest for inexpensive and rapid commercial production. However,t hey have decreased thermal stability. In an effort to increase thermal stability and explore framework flexibility, we have synthesized and characterized a series of analogs of the non-aluminosilicate RHO framework. All materials crystallize in the space group I23, ranging from a = 13.584-(2) A for Li-BePO RHO to a = 14.224(4) A for Ba-RbBeAsO RHO for hydrated phases. The extra framework cations are distributed over the double 8-ring, single 8-ring, and two single 6-ring sites. Partially and fully dehydrated phases were also studied for changes in framework stability. Predictive trends based on the type of cation exchanged into the framework were determined by {sup 9}Be and {sup 31}P MAS NMR. 50 refs., 8 figs., 6 tabs.

  2. Fast speciation of mercury in seawater by short-column high-performance liquid chromatography hyphenated to inductively coupled plasma spectrometry after on-line cation exchange column preconcentration.

    PubMed

    Jia, Xiao-Yu; Gong, Di-Rong; Han, Yi; Wei, Chao; Duan, Tai-Cheng; Chen, Hang-Ting

    2012-01-15

    A simple and fast method for trace speciation analysis of mercury (Hg(2+)), methylmercury (MeHg(+)) and ethylmercury (EtHg(+)) in seawater has been developed by short-column high-performance liquid chromatography hyphenated to inductively coupled plasma spectrometry (HPLC-ICP-MS) after on-line cation-exchange column (CEC) preconcentration. The analytes were firstly adsorbed on the CEC without any extraneous reagent, and then were eluted rapidly (within seconds) and completely with a very low concentration of l-cysteine solution, which provides the conveniency for the on-line coupling of the preconcentration method and detection technique. To our best knowledge, it is for the first time to employ the CEC preconcentration technique to trap all of the three mercury species simultaneously at their positive charged status for the purpose of speciation analysis. Under the optimized conditions, a very high preconcentration factor up to 1250 has been obtained with 30mL sample solution, which leads to the very low detection limits of 0.042ngL(-1) for Hg(2+), 0.016ngL(-1) for MeHg(+) and 0.008ngL(-1) for EtHg(+) (as Hg), respectively. With the established method, three seawater samples were also analyzed, and all the three mercury species have been found in each sample, albeit at a very low concentration. PMID:22265565

  3. Nearly 1000 Protein Identifications from 50 ng of Xenopus laevis Zygote Homogenate Using Online Sample Preparation on a Strong Cation Exchange Monolith Based Microreactor Coupled with Capillary Zone Electrophoresis.

    PubMed

    Zhang, Zhenbin; Sun, Liangliang; Zhu, Guijie; Cox, Olivia F; Huber, Paul W; Dovichi, Norman J

    2016-01-01

    A sulfonate-silica hybrid strong cation exchange monolith microreactor was synthesized and coupled to a linear polyacrylamide coated capillary for online sample preparation and capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) bottom-up proteomic analysis. The protein sample was loaded onto the microreactor in an acidic buffer. After online reduction, alkylation, and digestion with trypsin, the digests were eluted with 200 mM ammonium bicarbonate at pH 8.2 for CZE-MS/MS analysis using 1 M acetic acid as the background electrolyte. This combination of basic elution and acidic background electrolytes results in both sample stacking and formation of a dynamic pH junction. 369 protein groups and 1274 peptides were identified from 50 ng of Xenopus laevis zygote homogenate, which is comparable with an offline sample preparation method, but the time required for sample preparation was decreased from over 24 h to less than 40 min. Dramatically improved performance was produced by coupling the reactor to a longer separation capillary (∼100 cm) and a Q Exactive HF mass spectrometer. 975 protein groups and 3749 peptides were identified from 50 ng of Xenopus protein using the online sample preparation method. PMID:26670623

  4. Methanol sensing characteristics of conducting polypyrrole-silver nanocomposites

    NASA Astrophysics Data System (ADS)

    Kabir, L.; Mandal, S. K.

    2012-05-01

    Methanol sensing characteristics of conducting polypyrrole-silver nanocomposites are reported here. The nanocomposites are synthesized by wet chemical technique with different amount of silver loadings (5-15 mol%). The sensitivity of the nanocomposites upon exposure to gas molecules is critically dependent on the silver loadings and the concentration of the exposed gas. This is possibly instigated by the modified metal-polymer interface and the polar nature of the constituent metal and the exposed gas. Interaction of the alcohol gas with the polypyrrole chains in the presence of silver effectively determines the change in resistance and hence the sensitivity of the nanocomposites upon exposure to methanol. The adsorption of methanol molecules within the nanocomposites and the subsequent chemical reactions are studied by Fourier transform infrared (FTIR) spectroscopy.

  5. Nano-composite of poly(L-lactide) and halloysite nanotubes surface-grafted with L-lactide oligomer under microwave irradiation.

    PubMed

    Luo, Bing-Hong; Hsu, Chung-En; Li, Jian-Hua; Zhao, Liang-Feng; Liu, Ming-Xian; Wang, Xiao-Ying; Zhou, Chang-Ren

    2013-04-01

    In order to improve the bonding between halloysite nanotubes (HNTs) and poly(L-lactide) (PLLA), and hence to increase the mechanical properties of HNTs/PLLA nano-composite, HNTs were surface-grafted with PLLA under microwave irradiation and then blended with PLLA matrix. The optimal conditions for grafting polymerization are: irradiation time of 30 min, microwave power of 30 W and reaction temperature of 130 degrees C. The structure and properties of the surface-grafted HNTs (g-HNTs) were characterized by Fourier transformation infrared (FTIR), thermal gravimetric analysis (TGA), X-ray diffraction (XRD) and dynamic light scattering (DLS). Nano-composites of g-HNTs/PLLA and non-grafted HNTs/PLLA were subsequently evaluated in terms of crystallinity, dispersion, interfacial interaction, mechanical performance and cytocompatibility by polarized optical microscopy (POM), field scanning electron microscope (FESM), tensile testing and cell culture experiment. Results show that the grafted PLLA chains on the surfaces of HNTs, as inter-tying molecules, played an important role in improving the adhesive strength between the nanotubes and the polymer matrix. The enhanced interaction among g-HNTs and PLLA matrix resulted in a better tensile strength and modulus compared to the pristine PLLA and HNTs/PLLA. Cell culture results indicated that g-HNTs promoted both adhesion and proliferation of M3T3 fibroblasts on the g-HNTs/PLLA composite film. PMID:23621025

  6. Reaction kinetics for the solid state synthesis of the AlH3/MgCl2 nano-composite by mechanical milling.

    PubMed

    Duan, C W; Hu, L X; Sun, Y; Zhou, H P; Yu, H

    2015-09-14

    The process of mechanical milling has been proved to be a cost-effective way to synthesize the AlH3/MgCl2 nano-composite by using MgH2 and AlCl3 as reagents. However, so far there is no comprehensive knowledge of the kinetics of this process. In an effort to predict the reaction progress and optimize the milling parameters, the kinetics of the synthesis of the AlH3/MgCl2 nano-composite by mechanical milling of MgH2 and AlCl3 is experimentally investigated in the present work. The reaction progress or the transformation fraction upon milling for different times is evaluated using the isothermal hydrogen desorption test of the as-milled samples at 220 °C, which is much lower than the threshold temperature for the de-hydriding of the reagent MgH2 but enough for the de-hydriding of the as-synthesized nano-sized AlH3. The effects of milling parameters on the reaction kinetics as well as the underlying mechanism are discussed by referring to the mechanical energy input intensity, the vial temperature and the Gibbs free energy change for the reaction. Furthermore, it is found that the Johnson-Mehl-Avrami (JMA) model can well describe the kinetics theoretically. By fitting the experimental data with the JMA expression, the theoretical kinetics expressions, the equation parameters, and the activation energy are obtained. PMID:26256935

  7. Room-temperature solution-processed and metal oxide-free nano-composite for the flexible transparent bottom electrode of perovskite solar cells.

    PubMed

    Lu, Haifei; Sun, Jingsong; Zhang, Hong; Lu, Shunmian; Choy, Wallace C H

    2016-03-21

    The exploration of low-temperature and solution-processed charge transporting and collecting layers can promote the development of low-cost and large-scale perovskite solar cells (PVSCs) through an all solution process. Here, we propose a room-temperature solution-processed and metal oxide-free nano-composite composed of a silver nano-network and graphene oxide (GO) flawless film for the transparent bottom electrode of a PVSC. Our experimental results show that the amount of GO flakes play a critical role in forming the flawless anti-corrosive barrier in the silver nano-network through a self-assembly approach under ambient atmosphere, which can effectively prevent the penetration of liquid or gaseous halides and their corrosion against the silver nano-network underneath. Importantly, we simultaneously achieve good work function alignment and surface wetting properties for a practical bottom electrode by controlling the degree of reduction of GO flakes. Finally, flexible PVSC adopting the room-temperature and solution-processed nano-composite as the flexible transparent bottom electrode has been demonstrated on a polyethylene terephthalate (PET) substrate. As a consequence, the demonstration of our room-temperature solution-processed and metal oxide-free flexible transparent bottom electrode will contribute to the emerging large-area flexible PVSC technologies. PMID:26923479

  8. O-doped Si2Sb2Te5 nano-composite phase change material for application of chalcogenide random access memory.

    PubMed

    Zhang, Ting; Song, Zhitang; Liu, Bo; Wang, Feng; Feng, Songlin

    2009-02-01

    A method to prepare nano-composite phase change material was proposed and demonstrated by oxygen doping into Si2Sb2Te5 material. According to transmission electron microscope images, Si-Sb-Te-rich domains are separated from each other by SiOx-rich domains within the material. A proper dose of O-doping into Si2Sb2Te5 significantly reduces the grain size of the phase change material. Average size of Si-Sb-Te-rich domains is about 10 nm. Such separation will limit the phase-change to a relatively small volume. The reduction of grain size further results in the promotion of data retention and thermal stability of the material. Memory device based on O-doped Si2Sb2Te5 nano-composite phase change material, with a bottom electrode contact of 260 nm in diameter, was fabricated and characterized. The memory cell shows a better electrical performance compared with the Ge2Sb2Te5 based one. PMID:19441462

  9. Preparation and characterization of nano-composites with carbon nanotubes and core-shell type polyaniline for the conductive colloidal ink

    NASA Astrophysics Data System (ADS)

    Lee, Jungmin; Varadan, Vijay K.

    2012-04-01

    Printing method for electronics elements fabrication has attractive advantages such as low material consumption, high speed fabrication, and low temperature process. The stable conductive ink is the most important factor for the fabrication of printed electronics elements with high resolution. These materials are widely used as fillers in conductive inks; metal particles, conductive polymers, and carbon materials. Among these materials, the carbon nanotubes (CNTs) are extremely attractive filler for printed electronics due to its superior electrical properties, extra high mechanical properties, and excellent chemical stability. In this research, nano-composites which are composed of multi wall carbon nanotubes (MWCNTs) and polyaniline core-shell type particles were synthesized and formulated into electrically conductive colloidal inks. The poly(acrylonitrile-co-itaconic acid-co-methylacrylate) nanoparticles were used as cores. And this core was coated with polyaniline. The surface treatments for MWCNTs were applied to make the stable nano-composites. The experimental conditions were optimized to achieve high miscibility between MWCNTs and polyaniline coated particles. Their structure and surface morphology of the nanocomposites were characterized by Scanning Electron Microscopy. And four point probe automatic resistivity meter was used to measure the conductivities of the nanocomposites.

  10. Sulfur/graphitic hollow carbon sphere nano-composite as a cathode material for high-power lithium-sulfur battery.

    PubMed

    Shin, Eon Sung; Kim, Min-Seop; Cho, Won Il; Oh, Si Hyoung

    2013-01-01

    The intrinsic low conductivity of sulfur which leads to a low performance at a high current rate is one of the most limiting factors for the commercialization of lithium-sulfur battery. Here, we present an easy and convenient method to synthesize a mono-dispersed hollow carbon sphere with a thin graphitic wall which can be utilized as a support with a good electrical conductivity for the preparation of sulfur/carbon nano-composite cathode. The hollow carbon sphere was prepared from the pyrolysis of the homogenous mixture of the mono-dispersed spherical silica and Fe-phthalocyanine powder in elevated temperature. The composite cathode was manufactured by infiltrating sulfur melt into the inner side of the graphitic wall. The electrochemical cycling shows a capacity of 425 mAh g-1 at 3 C current rate which is more than five times larger than that for the sulfur/carbon black nano-composite prepared by simple ball milling. PMID:23914902

  11. Actuation properties of electrochemically driven polypyrrole free-standing films

    SciTech Connect

    Chiarelli, P.; De Rossi, D. |; Della Santa, A.; Mazzoldi, A.

    1994-12-31

    In this paper the authors report about investigations on coupled electrochemomechanical phenomena in polypyrrole (PPy) free-standing films. Quantitative measurements of isotonic length and relaxed elastic modulus changes are performed on PPy samples during cyclic voltammetry and square-wave amperometry. The link between dimensional and mechanical changes in the samples and doping salt exchange kinetics is investigated and a possible interpretation is proposed.

  12. Novel pH-sensitive films constructed from polypyrrole composites

    NASA Astrophysics Data System (ADS)

    Tsamouras, D.; Dalas, E.; Sakkopoulos, S.; Vitoratos, E.

    1993-11-01

    A new type of solid state chemiresistors sensitive to pH-changes is described. The chemical-sensitive layer consists of polypyrrole incorporated into a polyvinyl alcohol polymer matrix by polymerization under vacuum. Preliminary testing has shown these sensors to be stable in aqueous solutions at temperatures up to 50°C with response times in seconds. At 25°C the sensor sensitivity was 47Ω/pH. Interferences appear to be acceptably small.

  13. Polypyrrole coated magnetite nanoparticles from water based nanofluids

    NASA Astrophysics Data System (ADS)

    Turcu, R.; Pana, O.; Nan, A.; Craciunescu, I.; Chauvet, O.; Payen, C.

    2008-12-01

    The synthesis and characterization of hybrid structures obtained by coating Fe3O4 magnetic nanoparticles from water based nanofluid with a polypyrrole (PPy) layer are reported. The thin amorphous layer of polypyrrole surrounding the crystalline magnetic core was observed by HRTEM. The FTIR spectra of the nanocomposites show that the absorption bands characteristic for pyrrole ring vibrations significantly shifted to lower frequencies in the nanocomposite spectra, which indicates a higher degree of oxidation of the PPy shell covering the magnetite as compared with conventional PPy. The existence of superparamagnetism in the investigated nanocomposites is evidenced by the missing hysterezis loop in the magnetization versus applied magnetic field dependences. The comparison between the physical size of nanoparticles determined from TEM analysis and the magnetic size deduced from magnetization measurements is discussed. The surface modification of magnetite by polypyrrole coating results in an increase in the saturation magnetization and of the apparent magnetic diameter of the nanoparticles. This novel effect is attributed to a charge transfer process from the conducting polymer to the surface iron ions of magnetite, producing an increase in the surface contribution to the overall magnetic moment of the nanoparticles.

  14. CSA doped polypyrrole-zinc oxide thin film sensor

    NASA Astrophysics Data System (ADS)

    Chougule, M. A.; Jundale, D. M.; Raut, B. T.; Sen, Shashwati; Patil, V. B.

    2013-02-01

    The polypyrrole-zinc oxide (PPy-ZnO) hybrid sensor doped with different weight ratios of camphor sulphonic acid (CSA) were prepared by spin coating technique. These CSA doped PPy-ZnO hybrids were characterized by field emission scanning electron microscope (FESEM) and fourier transform infrared (FTIR) which proved the formation of polypyrrole, PPy-ZnO and the interaction between polypyrrole - ZnO (PPy-ZnO) hybrid with CSA doping. The gas sensing properties of the PPy-ZnO hybrid films doped with CSA have been studied for oxidizing (NO2) as well as reducing (H2S, NH3, CH4OH and CH3OH) gases at room temperature. We demonstrate that CSA doped PPy-ZnO hybrid films are highly selective to NO2 along with high-sensitivity at low concentration (80% to 100 ppm) and better stability, which suggested that the CSA doped PPy-ZnO hybrid films are potential candidate for NO2 detection at room temperature.

  15. Effect of Annealing on Thermal & Optical Properties of Polypyrrole

    NASA Astrophysics Data System (ADS)

    Saxena, Rashmi; Dixit, Manasvi; Sharma, Kananbala; Saxena, Narendra S.; Sharma, Thaneshwar P.

    2008-04-01

    Pure polypyrrole sample (S1) was synthesized by chemical oxidation method using NaOH as reducing agent in aqueous HCl medium. The polypyrrole pellet sample (S2) was then annealed at 200 °C for 4 hrs. The amorphous nature of both annealed and as- prepared polypyrrole samples was confirmed by XRD. FTIR spectra of both samples were taken, which indicate the significant change in annealed sample (S2) compared to as prepared sample. Temperature dependence of effective thermal conductivity of both samples (S1, S2) was studied by Transient plane source (TPS) technique. The effective thermal conductivity (λe) obtained for S1 & S2 exhibits a variation with temperature and a peak was observed for the two samples at 150 °C & 120 °C with a value 0.17 W/mK & 0.18 W/mK respectively. The shift of thermal conductivity peak of annealed sample towards the lower temperature side is explained on the basis of removal of voids and defects on annealing. The absorption spectra of these samples were recorded by USB-2000 spectrophotometer at room temperature in the wavelength range 300-800 nm. From the analysis of absorption spectra, optical band gap of S1 & S2 were determined. It was found that the values of optical band gap for sample S1 & S2 are 2.39 eV&2.24 eV respectively.

  16. Synthesis, sintering and characterization of Al2O 3-TiC nano-composites powders from carbon coated precursors

    NASA Astrophysics Data System (ADS)

    Kaga, Hisashi

    Synthesis, sintering and characterization of Al2O3-TiC nano-composite powders from carbon coated precursors were investigated. Degussa P-25 titanium dioxide, Cabot carbon black, and Alfa Aesar aluminum were the initial starting powders. Hydrocarbon gas (C3H6) was used as the carbon source for the carbon coated precursors. Analytical methods employed in this research were BET surface area measurement, X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), Vickers hardness tester, and differential scanning calorimetry (DSC). For Al2O3-TiC formation studies, three different types of precursors which are carbon coated TiO2/Al mixture, mixture of carbon coated TiO2 and Al, and standard mixture of TiO 2, Al, and carbon black were prepared to examine formation mechanism reaction. The carbon coated TiO2/Al mixture dramatically changed the reaction mechanism and produced high quality nanosize Al2O 3-TiC powders. XRD and BET results showed that the carbon coated TiO 2/Al synthesized at 1200°C had only Al2O3 and TiC phases with high surface area about 22m2/g which were formed via intermediate phases of Ti2O3 and Al 3Ti. TEM results showed that the produced Al2O3-TiC powders had fine particle size (20--80 nm), narrow particle size distribution, and freely agglomerated. DSC curve and XRD results of the carbon coated TiO 2/Al mixture also showed that there were two endothermic and three successive weak exothermic reactions because released heat was controlled by the carbon coating. Experimentally determined the first exothermic reaction 5Al + 3TiO 2 → Al2O3 + Ti2O3 + Al3Ti which was compared with theoretical explanation model and they were found to be in agreement. Sintering behavior of nano-size Al 2O3-TiC synthesized from carbon coated precursors was investigated in Al2O3-TiC-MgO system using pressureless sintering and hot-pressing methods. After pressureless sintering, MgO doped Al 2O3-20wt.%TiC resulted in 98% of theoretical

  17. Elaboration of ammonia gas sensors based on electrodeposited polypyrrole--cobalt phthalocyanine hybrid films.

    PubMed

    Patois, Tilia; Sanchez, Jean-Baptiste; Berger, Franck; Fievet, Patrick; Segut, Olivier; Moutarlier, Virginie; Bouvet, Marcel; Lakard, Boris

    2013-12-15

    The electrochemical incorporation of a sulfonated cobalt phthalocyanine (sCoPc) in conducting polypyrrole (PPy) was done, in the presence or absence of LiClO4, in order to use the resulting hybrid material for the sensing of ammonia. After electrochemical deposition, the morphological features and structural properties of polypyrrole/phthalocyanine hybrid films were investigated and compared to those of polypyrrole films. A gas sensor consisting in platinum microelectrodes arrays was fabricated using silicon microtechnologies, and the polypyrrole and polypyrrole/phthalocyanine films were electrochemically deposited on the platinum microelectrodes arrays of this gas sensor. When exposed to ammonia, polymer-based gas sensors exhibited a decrease in conductance due to the electron exchange between ammonia and sensitive polymer-based layer. The characteristics of the gas sensors (response time, response amplitude, reversibility) were studied for ammonia concentrations varying from 1 ppm to 100 ppm. Polypyrrole/phthalocyanine films exhibited a high sensitivity and low detection limit to ammonia as well as a fast and reproducible response at room temperature. The response to ammonia exposition of polypyrrole films was found to be strongly enhanced thanks to the incorporation of the phthalocyanine in the polypyrrole matrix. PMID:24209308

  18. Ag@polypyrrole: A highly efficient nanocatalyst for the N-alkylation of amines using alcohols.

    PubMed

    Mandi, Usha; Kundu, Sudipta K; Salam, Noor; Bhaumik, Asim; Islam, Sk Manirul

    2016-04-01

    We have synthesized Ag@polypyrrole nanomaterial by dispersing ultrafine silver nanoparticles (Ag NPs) over the organic polymer polypyrrole. The Ag@polypyrrole material has been characterized by powder X-ray diffraction (PXRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), electron paramagnetic resonance (EPR), Fourier transform infrared (FT-IR), ultraviolet-visible absorption (UV-vis) and atomic adsorption spectroscopy (AAS), and thermogravimetric analysis (TGA). The XRD pattern suggested the cubic crystalline phase of Ag NPs in Ag@polypyrrole. TEM image analysis revealed that silver nanoparticles are highly dispersed in the polymer matrix. The Ag@polypyrrole acts as an efficient and versatile heterogeneous nanocatalyst in the N-alkylation of amines using alcohols. The catalyst can be easily prepared, highly robust and reused several times without decrease in its catalytic activity. PMID:26809107

  19. Effects of UV radiation on the preparation of polypyrrole in the presence of hydrogen peroxide

    NASA Astrophysics Data System (ADS)

    Zhang, Shihu; Lv, Guowei; Wang, Guolong; Zhu, Kaiming; Yu, Demei; Shao, Jinyou

    2015-10-01

    Conductive polypyrrole was synthesized with hydrogen peroxide (H2O2) as the oxidant. To promote the polymerization of pyrrole, UV radiation was employed. The effects of UV radiation on the preparation of polypyrrole were investigated. The polymerization of pyrrole was conducted with the H2O2 concentration in the range of 0.12-0.96 M and the H2SO4 concentration in the range of 6.8×10-4-0.19 M. The structure characterization indicated that the product polypyrrole was overoxidized partly depending on the concentrations of H2SO4 and H2O2. The increase in H2O2 concentration led to a slight increase in the oxidation and overoxidation of polypyrrole, simultaneously. However, the increase in H2SO4 concentration effectively suppressed the overoxidation of polypyrrole. The morphology, conductivity and thermal stability of the products were also characterized.

  20. Development and validation of a UHPLC-MS/MS assay for colistin methanesulphonate (CMS) and colistin in human plasma and urine using weak-cation exchange solid-phase extraction.

    PubMed

    Zhao, Miao; Wu, Xiao-Jie; Fan, Ya-Xin; Guo, Bei-Ning; Zhang, Jing

    2016-05-30

    A rapid ultra high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) assay method was developed for determination of CMS and formed colistin in human plasma and urine. After extraction on a 96-well SPE Supra-Clean Weak Cation Exchange (WCX) plate, the eluents were mixed and injected into the UHPLC-MS/MS system directly. A Phonomenex Kinetex XB-C18 analytical column was employed with a mobile phase consisting of solution "A" (acetonitrile:methanol, 1:1, v/v) and solution "B" (0.1% formic acid in water, v/v). The flow rate was 0.4mL/min with gradient elution over 3.5min. Ions were detected in ESI positive ion mode and the precursor-product ion pairs were m/z 390.7/101.3 for colistin A, m/z 386.0/101.2 for colistin B, and m/z 402.3/101.2 for polymyxin B1 (IS), respectively. The lower limit of quantification (LLOQ) was 0.0130 and 0.0251mg/L for colistin A and colistin B in both plasma and urine with accuracy (relative error, %)<±12.6% and precision (relative standard deviation, %)<±10.8%. Stability of CMS was demonstrated in biological samples before and during sample treatment, and in the extract. This new analytical method provides high-throughput treatment and optimized quantification of CMS and colistin, which offers a highly efficient tool for the analysis of a large number of clinical samples as well as routine therapeutic drug monitoring. PMID:26970986

  1. Porous Ceramic Spheres From Cation Exchange Beads

    NASA Technical Reports Server (NTRS)

    Dynys, Fred

    2005-01-01

    This document is a slide presentation that examines the use of a simple templating process to produce hollow ceramic spheres with a pore size of 1 to 10 microns. Using ion exchange process it was determined that the method produces porous ceramic spheres with a unique structure: (i.e., inner sphere surrounded by an outer sphere.)

  2. Novel Li{sub 4}Ti{sub 5}O{sub 12}/Sn nano-composites as anode material for lithium ion batteries

    SciTech Connect

    Sivashanmugam, Arumugam; Gopukumar, Sukumaran; Thirunakaran, Ramasamy; Nithya, Chandrasekaran; Prema, Shanmuga

    2011-04-15

    Research highlights: {yields} It is a novel attempt on nano composites involving Li{sub 4}Ti{sub 5}O{sub 12} and Sn to use as an anode material for lithium ion batteries. {yields} Li{sub 4}Ti{sub 5}O{sub 12} was obtained by a solid state route and nano-Sn particles were derived from a chemical reduction process. {yields} These materials are characterized for their physical and electrochemical characteristics. {yields} Li{sub 4}Ti{sub 5}O{sub 12}/Sn composite delivers stable and enhanced discharge capacity of 200mAhg{sup -1} and does not exhibit any irreversible capacity. {yields} The present investigation brings out novel high performing composites for lithium ion battery -- Abstract: Li{sub 4}Ti{sub 5}O{sub 12}/Sn nano-composites have been prepared as anode material for lithium ion batteries by high-energy mechanical milling method. Structure of the samples has been characterized by X-ray diffraction (XRD), which reveals the formation of phase-pure materials. Scanning electron microscope (SEM) and transmission electron microscope (TEM) suggests that the primary particles are around 100 nm size. The local environment of the metal cations is confirmed by Fourier transform infrared (FT-IR) and the X-ray photoelectron spectroscopy (XPS) confirms that titanium is present in Ti{sup 4+} state. The electrochemical properties have been evaluated by galvanostatic charge/discharge studies. Li{sub 4}Ti{sub 5}O{sub 12}/Sn-10% composite delivers stable and enhanced discharge capacity of 200 mAh g{sup -1} indicates that the electrochemical performance of Li{sub 4}Ti{sub 5}O{sub 12}/Sn nano-composites is associated with the size and distribution of the Sn particles in the Li{sub 4}Ti{sub 5}O{sub 12} matrix. The smaller the size and more homogeneous dispersion of Sn particles in the Li{sub 4}Ti{sub 5}O{sub 12} matrix exhibits better cycling performance of Li{sub 4}Ti{sub 5}O{sub 12}/Sn composites as compared to bare Li{sub 4}Ti{sub 5}O{sub 12} and Sn particles. Further, Li{sub 4

  3. Room-temperature solution-processed and metal oxide-free nano-composite for the flexible transparent bottom electrode of perovskite solar cells

    NASA Astrophysics Data System (ADS)

    Lu, Haifei; Sun, Jingsong; Zhang, Hong; Lu, Shunmian; Choy, Wallace C. H.

    2016-03-01

    The exploration of low-temperature and solution-processed charge transporting and collecting layers can promote the development of low-cost and large-scale perovskite solar cells (PVSCs) through an all solution process. Here, we propose a room-temperature solution-processed and metal oxide-free nano-composite composed of a silver nano-network and graphene oxide (GO) flawless film for the transparent bottom electrode of a PVSC. Our experimental results show that the amount of GO flakes play a critical role in forming the flawless anti-corrosive barrier in the silver nano-network through a self-assembly approach under ambient atmosphere, which can effectively prevent the penetration of liquid or gaseous halides and their corrosion against the silver nano-network underneath. Importantly, we simultaneously achieve good work function alignment and surface wetting properties for a practical bottom electrode by controlling the degree of reduction of GO flakes. Finally, flexible PVSC adopting the room-temperature and solution-processed nano-composite as the flexible transparent bottom electrode has been demonstrated on a polyethylene terephthalate (PET) substrate. As a consequence, the demonstration of our room-temperature solution-processed and metal oxide-free flexible transparent bottom electrode will contribute to the emerging large-area flexible PVSC technologies.The exploration of low-temperature and solution-processed charge transporting and collecting layers can promote the development of low-cost and large-scale perovskite solar cells (PVSCs) through an all solution process. Here, we propose a room-temperature solution-processed and metal oxide-free nano-composite composed of a silver nano-network and graphene oxide (GO) flawless film for the transparent bottom electrode of a PVSC. Our experimental results show that the amount of GO flakes play a critical role in forming the flawless anti-corrosive barrier in the silver nano-network through a self

  4. Co-precipitation synthesis of nano-composites consists of zinc and tin oxides coatings on glass with enhanced photocatalytic activity on degradation of Reactive Blue 160 KE2B.

    PubMed

    Habibi, Mohammad Hossein; Mardani, Maryam

    2015-02-25

    Nano-composite containing zinc oxide-tin oxide was obtained by a facile co-precipitation route using tin chloride tetrahydrate and zinc chloride as precursors and coated on glass by Doctor Blade deposition. The crystalline structure and morphology of composites were evaluated by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). The XRD results showed peaks relative to zinc oxide with hexagonal wurtzite structure and tin oxide with tetragonal structure. FESEM observations showed that the nano-composite consisted of aggregates of particles with an average particle size of 18 nm. The photocatalytic activity of the pure SnO2, pure ZnO, ZnSnO3-Zn2SnO4 and ZnO-SnO2 nano-structure thin films was examined using the degradation of a textile dye Reactive Blue 160 (KE2B). ZnO-SnO2 nano-composite showed enhanced photo-catalytic activity than the pure zinc oxide and tin oxide. The enhanced photo-catalytic activity of the nano-composite was ascribed to an improved charge separation of the photo-generated electron-hole pairs. PMID:25265524

  5. Synthesis and characterization of ZnO:TiO2 nano composites thin films deposited on glass substrate by sol-gel spray coating technique

    NASA Astrophysics Data System (ADS)

    Sutanto, Heri; Nurhasanah, Iis; Hidayanto, Eko; Wibowo, Singgih; Hadiyanto

    2015-12-01

    In this work, (ZnO)x:(TiO2)1-x nano composites thin films, with x = 1, 0.75, 0.5, 0.25, and 0, have been prepared by sol-gel spray coating technique onto glass substrate. Pure TiO2 and ZnO thin films were synthesized from titanium isopropoxide-based and zinc acetate-based precursor solutions, respectively, whereas the composite films were obtained from the mixture of these solutions at the specific % vol ratios. The properties and performance of nano composite ZnO, TiO2 and ZnO:TiO2 thin films at different composition have been investigated. Ultraviolet - Visible (UV-Vis) Spectrophotometer and Scanning Electron Microscopy (SEM) were employed in order to get morphology and transmittance of thin films. Testing the ability of photocatalytic activity of obtained films was conducted on photodegradation of methylene blue (MB) dye and organic pollutants of wastewater under a 30 watt UV light irradiation, then testing BOD, COD and TPC were conducted. Using the Tauc model, the band-gap energy decreased from 3.12 eV to 3.02 eV for the sample with x = 1 and 0, respectively. This decrease occured along with the replacement of percentage of ZnO by TiO2 on the films. This decrease also reduced the minimum energy that required for electron excitation. Obtained thin films had nanoscale roughness level with range 3.64 to 17.30 nm. The film with x= 0 has the biggest removal percentage on BOD, COD and TPC mesurements with percentage 54.82%, 62.73% and 99.88%, respectively.

  6. Synthesis and characterization of ZnO:TiO{sub 2} nano composites thin films deposited on glass substrate by sol-gel spray coating technique

    SciTech Connect

    Sutanto, Heri Nurhasanah, Iis; Hidayanto, Eko; Wibowo, Singgih; Hadiyanto

    2015-12-29

    In this work, (ZnO){sub x}:(TiO{sub 2}){sub 1-x} nano composites thin films, with x = 1, 0.75, 0.5, 0.25, and 0, have been prepared by sol–gel spray coating technique onto glass substrate. Pure TiO{sub 2} and ZnO thin films were synthesized from titanium isopropoxide-based and zinc acetate-based precursor solutions, respectively, whereas the composite films were obtained from the mixture of these solutions at the specific % vol ratios. The properties and performance of nano composite ZnO, TiO{sub 2} and ZnO:TiO{sub 2} thin films at different composition have been investigated. Ultraviolet – Visible (UV-Vis) Spectrophotometer and Scanning Electron Microscopy (SEM) were employed in order to get morphology and transmittance of thin films. Testing the ability of photocatalytic activity of obtained films was conducted on photodegradation of methylene blue (MB) dye and organic pollutants of wastewater under a 30 watt UV light irradiation, then testing BOD, COD and TPC were conducted. Using the Tauc model, the band-gap energy decreased from 3.12 eV to 3.02 eV for the sample with x = 1 and 0, respectively. This decrease occured along with the replacement of percentage of ZnO by TiO{sub 2} on the films. This decrease also reduced the minimum energy that required for electron excitation. Obtained thin films had nanoscale roughness level with range 3.64 to 17.30 nm. The film with x= 0 has the biggest removal percentage on BOD, COD and TPC mesurements with percentage 54.82%, 62.73% and 99.88%, respectively.

  7. Use of the Simple Infiltrated Microstructure Polarization Loss Estimation (SIMPLE) model to describe the performance of nano-composite solid oxide fuel cell cathodes.

    PubMed

    Nicholas, Jason D; Wang, Lin; Call, Ann V; Barnett, Scott A

    2012-11-28

    Nano-composite Sm(0.5)Sr(0.5)CoO(3-δ) (SSC)-Ce(0.9)Gd(0.1)O(1.95) (GDC) and La(0.6)Sr(0.4)Co(0.8)Fe(0.2)O(3-δ) (LSCF)-GDC Solid Oxide Fuel Cell (SOFC) cathodes with various infiltrate loading levels were prepared through multiple nitrate solution infiltrations into porous GDC ionic conducting (IC) scaffolds. Microstructural analyses indicated that the average SSC and average LSCF hemispherical particle radii remained roughly constant, at 25 nm, across multiple infiltration-gelation-firing sequences. Comparisons between symmetric cell polarization resistance measurements and Simple Infiltrated Microstructure Polarization Loss Estimation (SIMPLE) model predictions showed that the SIMPLE model was able to predict the performance of heavily infiltrated SSC-GDC and LSCF-GDC cathodes with accuracies better than 55% and 70%, respectively (without the use of fitting parameters). Poor electronic conduction between mixed ionic electronic conducting (MIEC) infiltrate particles was found in lightly infiltrated cathodes. Since these electronic conduction losses were not accounted for by the SIMPLE model, larger discrepancies between the SIMPLE-model-predicted and measured polarization resistances were observed for lightly infiltrated cathodes. This work demonstrates that the SIMPLE model can be used to quickly determine the lowest possible polarization resistance of a variety of infiltrated MIEC on IC nano-composite cathodes (NCC's) when the NCC microstructure and an experimentally-applicable set of intrinsic MIEC oxygen surface resistances and IC bulk oxygen conductivities are known. Currently, this model is the only one capable of predicting the polarization resistance of heavily infiltrated MIEC on IC NCC's as a function of temperature, cathode thickness, nano-particle size, porosity, and composition. PMID:23060257

  8. A new high-throughput method utilizing porous silica-based nano-composites for the determination of partition coefficients of drug candidates.

    PubMed

    Yu, Chih H; Tam, Kin; Tsang, Shik C

    2011-09-01

    We show that highly porous silica-based nanoparticles prepared via micro-emulsion and sol-gel techniques are stable colloids in aqueous solution. By incorporating a magnetic core into the porous silica nano-composite, it is found that the material can be rapidly separated (precipitated) upon exposure to an external magnetic field. Alternatively, the porous silica nanoparticles without magnetic cores can be equally separated from solution by applying a high-speed centrifugation. Using these silica-based nanostructures a new high-throughput method for the determination of partition coefficient for water/n-octanol is hereby described. First, a tiny quantity of n-octanol phase is pre-absorbed in the porous silica nano-composite colloids, which allows an establishment of interface at nano-scale between the adsorbed n-octanol with the bulk aqueous phase. Organic compounds added to the mixture can therefore undergo a rapid partition between the two phases. The concentration of drug compound in the supernatant in a small vial can be determined by UV-visible absorption spectroscopy. With the adaptation of a robotic liquid handler, a high-throughput technology for the determination of partition coefficients of drug candidates can be employed for drug screening in the industry based on these nano-separation skills. The experimental results clearly suggest that this new method can provide partition coefficient values of potential drug candidates comparable to the conventional shake-flask method but requires much shorter analytical time and lesser quantity of chemicals. PMID:21780284

  9. Novel Germanium/Polypyrrole Composite for High Power Lithium-ion Batteries

    PubMed Central

    Gao, Xuanwen; Luo, Wenbin; Zhong, Chao; Wexler, David; Chou, Shu-Lei; Liu, Hua-Kun; Shi, Zhicong; Chen, Guohua; Ozawa, Kiyoshi; Wang, Jia-Zhao

    2014-01-01

    Nano-Germanium/polypyrrole composite has been synthesized by chemical reduction method in aqueous solution. The Ge nanoparticles were directly coated on the surface of the polypyrrole. The morphology and structural properties of samples were determined by X-ray diffraction, scanning electron microscopy and transmission electron microscopy. Thermogravimetric analysis was carried out to determine the polypyrrole content. The electrochemical properties of the samples have been investigated and their suitability as anode materials for the lithium-ion battery was examined. The discharge capacity of the Ge nanoparticles calculated in the Ge-polypyrrole composite is 1014 mAh g−1 after 50 cycles at 0.2 C rate, which is much higher than that of pristine germanium (439 mAh g−1). The composite also demonstrates high specific discharge capacities at different current rates (1318, 1032, 661, and 460 mAh g−1 at 0.5, 1.0, 2.0, and 4.0 C, respectively). The superior electrochemical performance of Ge-polypyrrole composite could be attributed to the polypyrrole core, which provides an efficient transport pathway for electrons. SEM images of the electrodes have demonstrated that polypyrrole can also act as a conductive binder and alleviate the pulverization of electrode caused by the huge volume changes of the nanosized germanium particles during Li+ intercalation/de-intercalation. PMID:25168783

  10. A new electroactive paper actuator using conducting polypyrrole

    NASA Astrophysics Data System (ADS)

    Deshpande, Shripad D.; Kim, Jaehwan; Yun, Seong R.

    2004-07-01

    The construction of electromechanical actuator has been achieved by using the conducting polypyrrole films deposition onto a gold-coated cellophane paper. This is probably the first report of this type of paper actuator. The conducting polypyrrole was electro-generated using either galvanostatic or potentiostatic conditions at 0.5 mA/cm2 current density or 0.7 volts applied potential. The two types of actuators were constructed namely: 1.Ppy/Cellophane bilayer 2. Ppy/ Cellophane paper /Ppy trilayer using electrochemical technique. These actuators showed a reversible and reproducible displacement in acetonitrile solution containing LiClO4 (1M). The maximum displacement of 9.1 mm was recorded for tri-layer device and 3.5 mm for bi-layer device in 1M LiClO4 acetonitrile solutions. The prepared actuator devices were investigated for their mechanical actuation in air medium. The actuation in air is comparatively less than in solution actuation, but still it showed significant movement in air also. The results obtained in acetonitrile solution containing 1M LiClO4 shows that the actuator requires very low excitation voltages of 0.2 MV m-1 at 0.5 Hz frequencies. The effect of humidity on the actuation properties was addressed. The humidity measurement was carried out between 60% to 95% humidity with the help of humidity-temperature controlled chamber. The resonating frequency of 3 Hz at 6 volts had shown 1.8 mm displacement at 95% humidity for gold-coated cellophane sample without polypyrrole.

  11. A simplified protein precipitation/mixed-mode cation-exchange solid-phase extraction, followed by high-speed liquid chromatography/mass spectrometry, for the determination of a basic drug in human plasma.

    PubMed

    Xue, Y-J; Akinsanya, J Billy; Liu, Jane; Unger, Steve E

    2006-01-01

    A simplified protein precipitation/mixed-mode cation-exchange solid-phase extraction (PPT/SPE) procedure has been investigated. A mixture of acetonitrile and methanol along with formic acid was used to precipitate plasma proteins prior to selectively extracting the basic drug. After vortexing and centrifugation, the supernatants were directly loaded onto an unconditioned Oasis MCX microElution 96-well extraction plate, where the protonated drug was retained on the negatively charged sorbent while interfering neutral lipids, steroids or other endogenous materials were washed away. Normal wash steps were deemed unnecessary and not used before sample elution. The sample extracts were analyzed under both conventional and high-speed liquid chromatography/tandem mass spectrometry (LC/MS/MS) conditions to examine the feasibility of the PPT/SPE procedure for human plasma sample clean-up. For the conventional LC/MS/MS method, chromatographic separation was achieved on a C18, 2.1 x 50 mm column with gradient elution (k' = 5.5). The mobile phase contained 0.1% formic acid in water and 0.1% formic acid in acetonitrile. For the high-speed LC/MS/MS method, chromatographic separation was achieved on a C18, 2.1 x 10 mm guard column with gradient elution (k' = 2.2, Rt = 0.26 min). The mobile phase contained 0.1% formic acid in water and 0.001% trifluoroacetic acid in acetonitrile. Detection for both conventional and high-speed LC/MS/MS methods was by positive ion electrospray tandem mass spectrometry on a ThermoElectron Finnigan TSQ Quantum Ultra, where enhanced resolution (RP 2000; 0.2 amu) was used for high-speed LC/MS/MS. The standard curve, ranging from 0.5 to 100 ng/mL, was fitted to a 1/x weighted quadratic regression model. This combined PPT/SPE procedure effectively eliminated time-consuming sorbent conditioning and wash steps, which are essential for a conventional mixed-mode SPE procedure, but retained the advantages of both PPT (removal of plasma proteins) and mixed

  12. Hybride magnetic nanostructure based on amino acids functionalized polypyrrole

    SciTech Connect

    Nan, Alexandrina Bunge, Alexander; Turcu, Rodica

    2015-12-23

    Conducting polypyrrole is especially promising for many commercial applications because of its unique optical, electric, thermal and mechanical properties. We report the synthesis and characterization of novel pyrrole functionalized monomers and core-shell hybrid nanostructures, consisting of a conjugated polymer layer (amino acids functionalized pyrrole copolymers) and a magnetic nanoparticle core. For functionalization of the pyrrole monomer we used several amino acids: tryptophan, leucine, phenylalanine, serine and tyrosine. These amino acids were linked via different types of hydrophobic linkers to the nitrogen atom of the pyrrole monomer. The magnetic core-shell hybrid nanostructures are characterized by various methods such as FTIR spectroscopy, transmission electron microscopy (TEM) and magnetic measurements.

  13. Gas Sensitivity Study of Polypyrrole Decorated Graphene Oxide Thick Film

    NASA Astrophysics Data System (ADS)

    Patil, Pritam; Gaikwad, Ganesh; Patil, Devidas Ramrao; Naik, Jitendra

    2016-04-01

    Polypyrrole (PPy) and graphene oxide (GO) nanocomposites were prepared by in situ polymerization method. The synthesized nanocomposites were characterized for current-voltage characteristic, Fourier transform infrared spectroscopy, X-ray diffraction and field emission scanning electron microscopy, which gave the evidence of the strong interaction between PPy nanofibers and GO nanosheets. The PPy/GO nanocomposites were used for the sensing of H2S, LPG, CO2 and NH3 gases respectively at room temperature. It was observed that PPy/GO nanocomposites with different GO weight ratios (5, 10 and 20 %) had better selectivity and sensitivity towards NH3 at room temperature.

  14. Characterization of electrochemically deposited polypyrrole using magnetoelastic material transduction elements

    NASA Technical Reports Server (NTRS)

    Ersoz, Arzu; Ball, J. Christopher; Grimes, Craig A.; Bachas, Leonidas G.

    2002-01-01

    Magnetoelastic alloy films have been used as a working electrode in an electrochemical cell. This material allows magnetic interrogation of electrochemical deposition. This technique was used to monitor the electrochemical deposition of polypyrrole by multisweep (CV) and potentiostatic methods. Since the determination of the mass-sensitive magnetoelastic film's resonance frequency is based on magnetic transduction, an inherent advantage of this method is that it requires no electrical connections other than the working lead of the potentiostat. Increases in pyrrole deposition correlated with a decrease in the peak resonance frequency of the magnetoelastic alloy. This technique provides a novel approach by which one can monitor electrochemical processes.

  15. Hybride magnetic nanostructure based on amino acids functionalized polypyrrole

    NASA Astrophysics Data System (ADS)

    Nan, Alexandrina; Bunge, Alexander; Turcu, Rodica

    2015-12-01

    Conducting polypyrrole is especially promising for many commercial applications because of its unique optical, electric, thermal and mechanical properties. We report the synthesis and characterization of novel pyrrole functionalized monomers and core-shell hybrid nanostructures, consisting of a conjugated polymer layer (amino acids functionalized pyrrole copolymers) and a magnetic nanoparticle core. For functionalization of the pyrrole monomer we used several amino acids: tryptophan, leucine, phenylalanine, serine and tyrosine. These amino acids were linked via different types of hydrophobic linkers to the nitrogen atom of the pyrrole monomer. The magnetic core-shell hybrid nanostructures are characterized by various methods such as FTIR spectroscopy, transmission electron microscopy (TEM) and magnetic measurements.

  16. A mathematical model for predicting cyclic voltammograms of electronically conductive polypyrrole

    NASA Technical Reports Server (NTRS)

    Yeu, Taewhan; Nguyen, Trung V.; White, Ralph E.

    1987-01-01

    Polypyrrole is an attractive polymer for use as a high-energy-density secondary battery because of its potential as an inexpensive, lightweight, and noncorrosive electrode material. A mathematical model to simulate cyclic voltammograms for polypyrrole is presented. The model is for a conductive porous electrode film on a rotating disk electrode (RDE) and is used to predict the spatial and time dependence of concentration, overpotential, and stored charge profiles within a polypyrrole film. The model includes both faradic and capacitance charge components in the total current density expression.

  17. A mathematical model for predicting cyclic voltammograms of electronically conductive polypyrrole

    NASA Technical Reports Server (NTRS)

    Yeu, Taewhan; Nguyen, Trung V.; White, Ralph E.

    1988-01-01

    Polypyrrole is an attractive polymer for use as a high-energy-density secondary battery because of its potential as an inexpensive, lightweight, and noncorrosive electrode material. A mathematical model to simulate cyclic voltammograms for polypyrrole is presented. The model is for a conductive porous electrode film on a rotating disk electrode (RDE) and is used to predict the spatial and time dependence of concentration, overpotential, and stored charge profiles within a polypyrrole film. The model includes both faradic and capacitance charge components in the total current density expression.

  18. Determination of diffusion coefficients in polypyrrole thin films using a current pulse relaxation method

    NASA Technical Reports Server (NTRS)

    Penner, Reginald M.; Vandyke, Leon S.; Martin, Charles R.

    1987-01-01

    The current pulse E sub oc relaxation method and its application to the determination of diffusion coefficients in electrochemically synthesized polypyrrole thin films is described. Diffusion coefficients for such films in Et4NBF4 and MeCN are determined for a series of submicron film thicknesses. Measurement of the double-layer capacitance, C sub dl, and the resistance, R sub u, of polypyrrole thin films as a function of potential obtained with the galvanostatic pulse method is reported. Measurements of the electrolyte concentration in reduced polypyrrole films are also presented to aid in the interpretation of the data.

  19. Amine-functionalized polypyrrole: Inherently cell adhesive conducting polymer.

    PubMed

    Lee, Jae Y; Schmidt, Christine E

    2015-06-01

    Electrically conducting polymers (CPs) have been recognized as novel biomaterials that can electrically communicate with biological systems. For their tissue engineering applications, CPs have been modified to promote cell adhesion for improved interactions between biomaterials and cells/tissues. Conventional approaches to improve cell adhesion involve the surface modification of CPs with biomolecules, such as physical adsorption of cell adhesive proteins and polycationic polymers, or their chemical immobilization; however, these approaches require additional multiple modification steps with expensive biomolecules. In this study, as a simple and effective alternative to such additional biomolecule treatment, we synthesized amine-functionalized polypyrrole (APPy) that inherently presents cell adhesion-supporting positive charges under physiological conditions. The synthesized APPy provides electrical activity in a moderate range and a hydrophilic surface compared to regular polypyrrole (PPy) homopolymers. Under both serum and serum-free conditions, APPy exhibited superior attachment of human dermal fibroblasts and Schwann cells compared to PPy homopolymer controls. Moreover, Schwann cell adhesion onto the APPy copolymer was at least similar to that on poly-l-lysine treated PPy controls. Our results indicate that amine-functionalized CP substrates will be useful to achieve good cell adhesion and potentially electrically stimulate various cells. In addition, amine functionality present on CPs can further serve as a novel and flexible platform to chemically tether various bioactive molecules, such as growth factors, antibodies, and chemical drugs. PMID:25294089

  20. Sequential growth for lifetime extension in biomimetic polypyrrole actuator systems

    NASA Astrophysics Data System (ADS)

    Sarrazin, J. C.; Mascaro, Stephen A.

    2015-04-01

    Electroactive polymers (EAPs) present prospective use in actuation and manipulation devices due to their low electrical activation requirements, biocompatibility, and mechanical performance. One of the main drawbacks with EAP actuators is a decrease in performance over extended periods of operation caused by over-oxidation of the polymer and general polymer degradation. Synthesis of the EAP material, polypyrrole with an embedded metal helix allows for sequential growth of the polymer during operation. The helical metal electrode acts as a scaffolding to support the polymer, and direct the 3-dimensional change in volume of the polymer along the axis of the helix during oxidative and reductive cycling. The metal helix also provides a working metal electrode through the entire length of the polymer actuator to distribute charge for actuation, as well as for sequential growth steps during the lifetime of operation of the polymer. This work demonstrates the method of sequential growth can be utilized after extended periods of use to partially restore electrical and mechanical performance of polypyrrole actuators. Since the actuation must be temporarily stopped to allow for a sequential growth cycle to be performed and reverse some of the polymer degradation, these actuator systems more closely mimic natural muscle in their analogous maintenance and repair.

  1. Morphology and electrical properties of template-synthesized polypyrrole nanocylinders

    NASA Astrophysics Data System (ADS)

    Mativetsky, J. M.; Datars, W. R.

    2002-11-01

    Polypyrrole nanocylinders were fabricated by chemically synthesizing polypyrrole within the pores of nanoporous polycarbonate particle track-etched membranes. The morphology of the nanostructures was characterized by transmission electron microscopy and scanning electron microscopy. The nanocylinders were observed to be cigar-shaped, with the diameter at the center being up to 2.5 times the diameter at the ends. The electrical conductivity of the nanocylinders was measured by leaving the nanocylinders embedded in the insulating template membrane and measuring the trans-membrane resistance. The cigar-like shape of the nanocylinders was taken into account in calculating the conductivity. Contrary to previous reports, the smallest diameter nanocylinders exhibited a slightly lower conductivity relative to the larger diameter nanocylinders. The temperature dependence of the resistance and magnetoresistance was in accordance with Mott variable range hopping at temperatures above 5±1 K and Efros-Shklovskii variable range hopping at temperatures below 5±1 K. Based on the measurements in the Mott regime, the localization length, the density of states at the Fermi energy, and the temperature dependence of the average hopping distance were calculated.

  2. Strong and electrically conductive nanopaper from cellulose nanofibers and polypyrrole.

    PubMed

    Lay, Makara; Méndez, J Alberto; Delgado-Aguilar, Marc; Bun, Kim Ngun; Vilaseca, Fabiola

    2016-11-01

    In this work, we prepare cellulose nanopapers of high mechanical performance and with the electrical conductivity of a semiconductor. Cellulose nanofibers (CNF) from bleached softwood pulp were coated with polypyrrole (PPy) via in situ chemical polymerization, in presence of iron chloride (III) as oxidant agent. The structure and morphology of nanopapers were studied, as well as their thermal, mechanical and conductive properties. Nanopaper from pure CNF exhibited a very high tensile response (224MPa tensile strength and 14.5GPa elastic modulus). The addition of up to maximum 20% of polypyrrole gave CNF/PPy nanopapers of high flexibility and still good mechanical properties (94MPa strength and 8.8GPa modulus). The electrical conductivity of the resulting CNF/PPy nanopaper was of 5.2 10(-2)Scm(-1), with a specific capacitance of 7.4Fg(-1). The final materials are strong and conductive nanopapers that can find application as biodegradable flexible thin-film transistor (TFT) or as flexible biosensor. PMID:27516283

  3. Structure, electrochemical properties and capacitance performance of polypyrrole electrodeposited onto 1-D crystals of iridium complex

    NASA Astrophysics Data System (ADS)

    Wysocka-Żołopa, Monika; Winkler, Krzysztof

    2015-12-01

    Composites of polypyrrole and one-dimensional iridium complex crystals [(C2H5)4N]0.55[IrCl2(CO)2] were prepared by in situ two-step electrodeposition. Initially, iridium complex crystals were formed during [IrCl2(CO)2]- complex oxidation. Next, pyrrole was electropolymerized on the surface of the iridium needles. The morphology of the composite was investigated by scanning and transmission electron microscopy. At positive potentials, the iridium complex crystals and the polypyrrole were oxidized. In aprotic solvents, oxidation of the iridium complex crystals resulted in their dissolution. In water containing tetra(n-butyl)ammonium chlorides, the 1-D iridium complex crystals were reversibly oxidized. The product of the iridium complex oxidation remained on the electrode surface in crystalline form. The iridium complex needles significantly influenced the redox properties of the polymer. The polypyrrole involved electrode processes become more reversible in presence of crystals of iridium complex. The current of polypyrrole oxidation was higher compared to that of pure polypyrrole and the capacitance properties of the polymer were significantly enhanced. A specific capacitance as high as 590 F g-1 was obtained for a composite of polypyrrole and 1-D crystals of the iridium complex in water containing tetra(n-butyl)ammonium chloride. This value is approximately twice as high as the capacitance of the pure polymer deposited onto the electrode surface.

  4. Enhanced Conductivity and Electrochemical Performance of Electrode Material Based on Multifunctional Dye Doped Polypyrrole.

    PubMed

    Zang, Limin; Qiu, Jianhui; Yang, Chao; Sakai, Eiichi

    2016-03-01

    Polypyrrole were prepared via in-situ chemical oxidative polymerization in the presence of multisulfonate acid dye (acid violet 19). In this work, acid violet 19 could play the role as dopant, surfactant and physical cross-linker for pyrrole polymerization, and had impact on the morphology, dispersion stability, thermal stability, electrical conductivity and electrochemical behavior of the samples. The thermal stability of the dye doped polypyrrole was enhanced than pure polypyrrole due to the strong interactions between polypyrrole and acid violet 19. The dispersion stability of the samples in water was also improved by incorporating an appropriate amount of acid violet 19. The sample with 20% of acid violet 19 showed granular morphology with the smallest diameter of -50 nm and possessed the maximum electrical conductivity of 39.09 S/cm. The as-prepared multifunctional dye doped polypyrrole samples were used to fabricate electrodes and exhibited a mass specific capacitance of 379-206 F/g in the current density range of 0.2-1.0 A/g. The results indicated that the multifunctional dye could improve the performances of polypyrrole as electrode material for supercapacitors. PMID:27455670

  5. Sol-Gel derived Sb-doped SnO II/SiO II nano-composite thin films for gas sensors

    NASA Astrophysics Data System (ADS)

    Gu, Zhengtian; Liang, Peihui; Zhang, Weiqing

    2006-05-01

    Sb-doped SnO II/SiO II nano-composite thin films prepared by sol-gel dip-coating method have been studied. By using X-ray diffraction (XRD), atomic force microscopy (AFM) and Fourier transform infrared (FTIR) spectroscopy, detailed investigation on the structure and morphology of the films has shown the crystalline grain size of Sb-doped SnO II/SiO II thin films is about 34nm, with larger specific surface area and duty porosity, which is fit for gas-sensing materials. The adulteration of SiO II particles leads to the condensation of Sn-OH and the strengthening of gel network, and improve the adhesion of the films. In addition, the optical properties of the thin films were studied by UV-Vis spectra and p-polarized light reflectance angular spectrum. The results showthat the optical transmissivity of Sb-doped SnO II/SiO II thin films is higher, near 95% in visible spectrum range, the measured optical gap is found equal to 3.67eV, also the films take on smaller refractive index and extinction coefficient compared with those of the SnO II and Sb:SnO II films, which is compatible with the semiconductor substrate in the solar cell. Further, the gas-sensing test was made to three kinds of gas C 3H 8, C IIH 5OH and NH 3 in our novel high sensitive scheme for optical film sensors. The results indicate that Sb doping to SnO II films greatly improves the gas sensitivity to C IIH 5OH, and the gas sensitivity of Sb:SnO II/SiO II nano-composite thin films are higher than that of Sb:SnO II thin films. The detection sensitivity of this optical film sensor is available to 10 -1ppm provided that the resolution of reflectance ratio is 10 -2.

  6. Use of nano-composite component to improve the conductivity and mechanical properties of Li{sub 2}SO{sub 4}-Al{sub 2}O{sub 3} solid electrolyte

    SciTech Connect

    Melnik, Juri; An Weizhu; Wei Guolin; Luo Jingli . E-mail: jingli.luo@ualberta.ca; Sanger, Alan R.; Chuang, Karl T.

    2006-10-12

    The microstructure, density, and conductivity of Li{sub 2}SO{sub 4} ion-conducting membranes incorporating nano-composite Li{sub 2}SO{sub 4}-Al{sub 2}O{sub 3} prepared using a sol-gel technique are superior to membranes having the same bulk composition prepared from mixtures of lithium sulfate and fine alumina powder. Properties of membranes made from the nano-composite material depend on both the overall composition and the preparative parameters. The relationships between preparative parameters, microstructure, and properties have been determined, from which we have found the optimum lithium sulfate content and thermal treatment parameters for manufacture of membranes with minimum gas permeability and maximum ionic conductivity.

  7. Immobilization of a novel cold active esterase onto Fe3O4∼cellulose nano-composite enhances catalytic properties.

    PubMed

    Rahman, Mohammad Asadur; Culsum, Umma; Kumar, Ashok; Gao, Haofeng; Hu, Nan

    2016-06-01

    A novel esterase, EstH was cloned, purified and characterized from the marine bacterium Zunongwangia sp. The purified EstH showed optimum activity at 30°C and pH 8.5 with ∼50% of original activity at 0°C. EstH was stable in high salt conditions (0-4.5M NaCl). To improve the characteristics and explore the possibilities for application, a new immobilization matrix, Fe3O4∼cellulose nano-composite, was prepared and was characterized by Fourier Transform Infrared Spectroscopy (FTIR) and Scanning Electron Microscope (SEM). Interestingly the optimal temperature of immobilized EstH elevated to 35°C. Compared to its free form, immobilized EstH showed better temperature stability (48.5% compared to 22.40% at 50°C after 30min), prolonged half-life (32h compared to 18h), higher storage stability (∼71% activity compared to ∼40% after 50days of storage), improved pH tolerance (∼73% activity at pH 4 and 10), and, more importantly, reusability (∼50% activity after 8 repetitive cycles of usage). Enzyme kinetics showed an increase in the Vmax (from 35.76 to 51.14μM/min) and Kcat (from 365s(-1) to 520s(-1)) after immobilization. The superior catalytic properties of immobilized EstH suggest its great potential in biotechnology and industrial processes. PMID:26976070

  8. Solution combustion synthesis of CeO{sub 2}-CeAlO{sub 3} nano-composites by mixture-of-fuels approach

    SciTech Connect

    Aruna, S.T.; Kini, N.S. Rajam, K.S.

    2009-04-02

    Nano-composites of CeO{sub 2}-CeAlO{sub 3} are synthesised by solution combustion method employing (a) urea and (b) a mixture of urea and glycine as fuels with corresponding metal nitrates. The as-prepared powders are all nano-sized (5-30 nm) and the same is confirmed by broadening of the X-ray diffraction peaks and transmission electron microscopy. A starting composition of Ce:Al in the atomic ratio 4:6 gives rise to different phases depending on the fuel being used for combustion. When urea alone is used as fuel, nano-crystalline CeO{sub 2} phase is formed with Al{sub 2}O{sub 3} being in the amorphous state. When the mixture of fuels is used, a mixture of nano-sized CeO{sub 2} and CeAlO{sub 3} phases is obtained. However, upon sintering at 1400 deg. C in air, the stable phases CeO{sub 2} and {alpha}-Al{sub 2}O{sub 3} are formed in both the cases. Combustion synthesis using mixture-of-fuels is proposed to be a route to stabilise low oxidation compounds such as CeAlO{sub 3}.

  9. Modeling the Break-up of Nano-particle Clusters in Aluminum- and Magnesium-Based Metal Matrix Nano-composites

    NASA Astrophysics Data System (ADS)

    Manoylov, Anton; Bojarevics, Valdis; Pericleous, Koulis

    2015-07-01

    Aluminum- and magnesium-based metal matrix nano-composites with ceramic nano-reinforcements promise low weight with high durability and superior strength, desirable properties in aerospace, automobile, and other applications. However, nano-particle agglomerations lead to adverse effects on final properties: large-size clusters no longer act as dislocation anchors, but instead become defects; the resulting particle distribution will be uneven, leading to inconsistent properties. To prevent agglomeration and to break-up clusters, ultrasonic processing is used via an immersed sonotrode, or alternatively via electromagnetic vibration. A study of the interaction forces holding the nano-particles together shows that the choice of adhesion model significantly affects estimates of break-up force and that simple Stokes drag due to stirring is insufficient to break-up the clusters. The complex interaction of flow and co-joint particles under a high frequency external field (ultrasonic, electromagnetic) is addressed in detail using a discrete-element method code to demonstrate the effect of these fields on de-agglomeration.

  10. In situ injectable nano-composite hydrogel composed of curcumin, N,O-carboxymethyl chitosan and oxidized alginate for wound healing application.

    PubMed

    Li, Xingyi; Chen, Shuo; Zhang, Binjun; Li, Mei; Diao, Kai; Zhang, Zhaoliang; Li, Jie; Xu, Yu; Wang, Xianhuo; Chen, Hao

    2012-11-01

    In this paper, an in situ injectable nano-composite hydrogel composed of curcumin, N,O-carboxymethyl chitosan and oxidized alginate as a novel wound dressing was successfully developed for the dermal wound repair application. Nano-curcumin with improved stability and similar antioxidant efficiency compared with that of unmodified curcumin was developed by using methoxy poly(ethylene glycol)-b-poly(ε-caprolactone) copolymer (MPEG-PCL) as carrier followed by incorporating into the N,O-carboxymethyl chitosan/oxidized alginate hydrogel (CCS-OA hydrogel). In vitro release study revealed that the encapsulated nano-curcumin was slowly released from CCS-OA hydrogel with the diffusion-controllable manner at initial phase followed by the corrosion manner of hydrogel at terminal phase. In vivo wound healing study was performed by injecting hydrogels on rat dorsal wounds. Histological study revealed that application of nano-curcumin/CCS-OA hydrogel could significantly enhance the re-epithelialization of epidermis and collagen deposition in the wound tissue. DNA, protein and hydroxyproline content in wound tissue from each group were measured on 7th day of post wounding and the results also indicated that combined using nano-curcumin and CCS-OA hydrogel could significantly accelerate the process of wound healing. Therefore, all these results suggested that the developed nano-curcumin/CCS-OA hydrogel as a promising wound dressing might have potential application in the wound healing. PMID:22903048

  11. Rheological properties of PP/CaCO3 micron-nano composite blends processing based on elongation rheology via vane extruder

    NASA Astrophysics Data System (ADS)

    Benhao, Kang; Rongyuan, Chen; Guizhen, Zhang; Zhitao, Yang; Jinping, Qu

    2016-03-01

    This work aimed to study, for the first time, the rheological properties of the melt blending of PP/micron-CaCO3 and PP/nano-CaCO3 composite processing based on elongation rheology by a novel vane extruder to toughen PP. The rheological behavior of the blends was studied by capillary rheometer. The results show that: PP/CaCO3 Micron-nano copolymer blends are pseudo plastic fluid. The apparent viscosity initially increases with the increasing of feller. The change of the apparent viscosity also depends on the filler type which proves difference when the blends are on the low shear rate. When the shear rate is low, the apparent shear viscosity of micron-nano composite material is more sensitive to shear rate. For PP/micron-CaCO3 composite blend, the non-Newtonian index shows a trend of gradually increasing. In PP/nano-CaCO3 composite blend, the non-Newtonian index changed little in general with the increase of nano-filler content.

  12. High-power lithium ion batteries based on preorganized necklace type Li4Ti5O12/VACNT nano-composites

    NASA Astrophysics Data System (ADS)

    Pawlitzek, Fabian; Pampel, Jonas; Schmuck, Martin; Althues, Holger; Schumm, Benjamin; Kaskel, Stefan

    2016-09-01

    Li4Ti5O12 as anode material for high power Li+-ion batteries is very promising due to its unique electronic properties. However, the lack of electronic conductivity as well as the low Li+-ion diffusion coefficient are major drawbacks in achieving high power densities. In this work, therefore, we prepared a nano-composite consisting of vertically aligned carbon nanotube arrays decorated with in-situ grown necklace type Li4Ti5O12 nanoparticles. Owing to this structure the electrodes exhibit outstanding rate performances with specific capacities of 110 mAh g-1 up to 300C and cycling performance with high capacity retention of 97% after 500 cycles at 10C. Thus, the combination of short Li+-ion diffusion distances within Li4Ti5O12 particles, remarkable electronic conductivity by carbon nanotubes directly grown on the current collector as well as a high contact surface area due to an open pore geometry is essential in achieving high power Li4Ti5O12 anodes.

  13. Effect of sintering in ball-milled K{sub 2}Bi{sub 8}Se{sub 13} thermoelectric nano-composites

    SciTech Connect

    Hatzikraniotis, E.; Ioannou, M.; Chrissafis, K.; Chung, D.Y.; Paraskevopoulos, K.M.; Kyratsi, Th.

    2012-09-15

    K{sub 2}Bi{sub 8}Se{sub 13} has many attractive features for thermoelectric applications. Recently, K{sub 2}Bi{sub 8}Se{sub 13}-based nanocomposite materials, consisting of nano-crystalline, micro-crystalline and amorphous phases, have been fabricated based on powder technology techniques. The Seebeck coefficient has been enhanced while the thermal conductivity has been decreased presenting, thus, interesting behavior. The behavior of the materials under heat treatment conditions is now of interest, as the application of sintering process is necessary for the development of thermoelectric modules. In this work, the crystallization of the K{sub 2}Bi{sub 8}Se{sub 13}-based nano-composites is studied using Differential Scanning Calorimetry. The results show that crystallization follows a multiple-step process with different activation energies. The thermoelectric properties are also discussed in the range that crystallization occurs. - Graphical Abstract: {beta}-K{sub 2}Bi{sub 8}Se{sub 13}-based nanocomposites follow a multiple-step crystallization process. Highlights: Black-Right-Pointing-Pointer K{sub 2}Bi{sub 8}Se{sub 13}-based composites consisting of nanocrystalline and amorphous phases. Black-Right-Pointing-Pointer Sintering results multiple-step crystallization with variable activation energies. Black-Right-Pointing-Pointer Thermoelectric properties follow a step-like behavior during sintering. Black-Right-Pointing-Pointer Properties are attributed to the strain relaxation, nucleation and grain growth.

  14. Enhanced conversion efficiency in dye-sensitized solar cells based on bilayered nano-composite photoanode film consisting of TiO2 nanoparticles and nanofibers.

    PubMed

    Du, P F; Song, L X; Xiong, J

    2014-06-01

    Novel TiO2 nanoparticles/nanofibers (NPs/NFs) bilayered nano-composite photoanode film for dye-sensitized solar cells (DSSCs) was fabricated through the combination of spin-coating and electrospinning. The NPs and NFs layers have complementary roles. The underlaid spin-coated NPs layer provides the photoanode film with higher specific surface area for dye adsorption and improved adhesion to conductive glass substrate. The overlaid electrospun NFs layer endows the photoanode film with better dye-loading and light-harvesting capabilities due to its porous meshwork structure. And the NFs layer also offers larger pore volume, which can facilitate the electrolyte diffusion and the activity regeneration of dye sensitizers. As a result, the electron transport is accelerated while the charge recombination is suppressed. Ascribing to the synergic effect of the NPs and NFs layers, the TiO2 NPs/NFs-based DSSCs achieve a conversion efficiency of 4.46%, which is nearly 14% higher than that of the pure TiO2 NPs-based ones. PMID:24738365

  15. Preparation of monodisperse polystyrene/silica core-shell nano-composite abrasive with controllable size and its chemical mechanical polishing performance on copper

    NASA Astrophysics Data System (ADS)

    Zhang, Lei; Wang, Haibo; Zhang, Zefang; Qin, Fei; Liu, Weili; Song, Zhitang

    2011-11-01

    Monodisperse silica-coated polystyrene (PS) nano-composite abrasives with controllable size were prepared via a two-step process. Monodisperse positively charged PS colloids were synthesized via polymerization of styrene by using a cationic initiator. In the subsequent coating process, silica formed shell on the surfaces of core PS particles via the ammonia-catalyzed hydrolysis and condensation of tetraethoxysilane. Neither centrifugation/water wash/redispersion cycle process nor surface modification or addition surfactant was needed in the whole process. The morphology of the abrasives was characterized by scanning electron microscope. Transmission electron microscope and energy dispersive X-ray analysis results indicated that silica layer was successfully coated onto the surfaces of PS particles. Composite abrasive has a core-shell structure and smooth surface. The chemical mechanical polishing performances of the composite abrasive and conventional colloidal silica abrasive on blanket copper wafers were investigated. The root mean square roughness decreases from 4.27 nm to 0.56 nm using composite abrasive. The PS/SiO2 core-shell composite abrasives exhibited little higher material removal rate than silica abrasives.

  16. Chitosan mediated synthesis of core/double shell ternary polyaniline/Chitosan/cobalt oxide nano composite-as high energy storage electrode material in supercapacitors

    NASA Astrophysics Data System (ADS)

    Vellakkat, Mini; Hundekkal, Devendrappa

    2016-01-01

    Nanostructured ternary composite of polyaniline (PANI), Co3O4 nanoparticles, and Chitosan (CS) has been prepared by an in situ chemical oxidation method, and the nanocomposites (CPAESCO) were used as supercapacitor electrodes. The Co3O4 nanoparticles are uniformly coated with CS and PANI layers in it. Different techniques (Fourier transform infrared spectrophotometry, x-ray diffraction, thermal gravimetric analysis, UV-visible spectroscopy, scanning electron microscopy, transmission electron microscopy and electro chemical analysis-cyclic voltammetry, galvanostatic charge/discharge (GCD), and electrochemical impedance spectroscopy) were used to analyse the optical, structural, thermal, chemical and supercapacitive aspects of the nanocomposites. Core/double shell ternary composite electrode exhibits significantly increased specific capacitance than PANI/Co3O4 or PANI/CS binary composites in supercapacitors. The ternary nanocomposite with 40% nanoparticle exhibits a highest specific capacitance reaching 687 F g-1, Energy density of (95.42 Wh kg-1 at 1 A g-1) and power density of (1549 W kg-1 at 3 A g-1) and outstanding cycling performance, with, 91% capacitance retained over 5000 cycles. It is found that this unique bio compatible nano composite with synergy is a new multifunctional material which will be useful in the design of supercapacitor electrodes and other energy conversion devices too.

  17. Implications of Degree of Thermal Shocks on Flexural Properties of Cu-Al2O3 Micro- and Nano-composites

    NASA Astrophysics Data System (ADS)

    Dash, K.; Ray, B. C.

    2016-01-01

    This investigation reports the effect of thermal shock of different gradients, i.e., immediate transition from high temperature to cryogenic environment and vice versa on the flexural properties of Al2O3 particulate reinforced Cu metal matrix micro- and nano-composites fabricated by powder metallurgy route. The specimens were also thermally conditioned at high as well as sub-zero temperatures separately. The specimens were subjected to 3-point flexural test followed by fractography, and the fracture micro-characteristics were studied under field emission scanning electron microscopy and transmission electron microscopy to predict the dislocation behavior under induced thermal stresses and mismatch. The degree of improvement in flexural strength is higher for the composites experiencing lower degree of thermal shock, i.e., improvement in flexural strength is higher for a thermal shock of 80 °C than for 160 °C temperature gradients. Particle pull-out, crack entrapment, and physical outgripping of alumina particles act as the operative mechanisms during fracture of thermally shocked composites.

  18. Stability of polypyrrole soft actuators in ionic liquids

    NASA Astrophysics Data System (ADS)

    Kaneto, Keiicgi; Takashima, Wataru

    2012-04-01

    Characteristics of electrochemomechanical deformation (ECMD) of polypyrrole films using ionic liquids are reported. The PPy film prepared by electrodeposition in an ionic liquid (1-Butyl-1-methylpyrrolidinium bis(trifluorometylsulfonyl)imide, BMPTFSI) was compact and high density. The other film prepared from LiTSFI/methyl benzoate and dimethyl phthalate mixed solvents was porous and low density. Both films demonstrated a stable ECMD in the ionic liquid. The strain of ECMD was 3-5% and superimposed on a creeping, showing a typical behaviour of cation movement. The Strains of ECMD in both films operated in a mixed electrolyte of BMPTFSI and propylene carbonate were enhanced up to 17- 25 %, showing anion movement. However, the large strain decreased upon several electrochemical cycles. The results were discussed in terms of swelling of the PPy film by solvents and loss of electrochemical activity.

  19. Effects of Ultramicroelectrode Dimensions on the Electropolymerization of Polypyrrole

    SciTech Connect

    Fletcher, Benjamin L; Fern, Jared T.; Rhodes, Kevin; McKnight, Timothy E; Fowlkes, Jason Davidson; Retterer, Scott T; Keffer, David J.; Simpson, Michael L; Doktycz, Mitchel John

    2009-01-01

    Anode geometry can significantly affect the electrochemical synthesis of conductive polymers. Here, the effects of anode dimensions on the electropolymerization of pyrrole are investigated. Band microelectrodes were prepared with widths ranging from 2 to 500 {micro}m. The anode dimension has a significant effect on the resulting thickness of polymer film. The electropolymerization process deviates significantly from that predicted by simple mass transfer considerations when electrode dimensions are less than {approx}20 {micro}m. Polymer film thickness is thinner than expected when electrode dimensions become less than {approx}10 {micro}m. A simple mathematical model was derived to explain the observed effects of anode dimensions on the polymerization process. Simulation results confirm that diffusive loss of reaction intermediates accounts for the observed experimental trends. The described simulation facilitates understanding of the electropolymerization processes and approaches to the controlled deposition of polypyrrole, particularly at the submicron scale, for microelectromechanical systems and biomedical applications.

  20. Electrochemical deposition of conductive and adhesive polypyrrole-dopamine films

    PubMed Central

    Kim, Semin; Jang, Lindy K.; Park, Hyun S.; Lee, Jae Young

    2016-01-01

    Electrode surfaces have been widely modified with electrically conductive polymers, including polypyrrole (PPY), to improve the performance of electrodes. To utilize conductive polymers for electrode modification, strong adhesion between the polymer films and electrode substrates should be ensured with high electrical/electrochemical activities. In this study, PPY films were electrochemically polymerized on electrodes (e.g., indium tin oxide (ITO)) with dopamine as a bio-inspired adhesive molecule. Efficient and fast PPY electrodeposition with dopamine (PDA/PPY) was found; the resultant PDA/PPY films exhibited greatly increased adhesion strengths of up to 3.7 ± 0.8 MPa and the modified electrodes had electrochemical impedances two to three orders of magnitude lower than that of an unmodified electrode. This electrochemical deposition of adhesive and conductive PDA/PPY offers a facile and versatile electrode modification for various applications, such as biosensors and batteries. PMID:27459901

  1. Electrochemical deposition of conductive and adhesive polypyrrole-dopamine films.

    PubMed

    Kim, Semin; Jang, Lindy K; Park, Hyun S; Lee, Jae Young

    2016-01-01

    Electrode surfaces have been widely modified with electrically conductive polymers, including polypyrrole (PPY), to improve the performance of electrodes. To utilize conductive polymers for electrode modification, strong adhesion between the polymer films and electrode substrates should be ensured with high electrical/electrochemical activities. In this study, PPY films were electrochemically polymerized on electrodes (e.g., indium tin oxide (ITO)) with dopamine as a bio-inspired adhesive molecule. Efficient and fast PPY electrodeposition with dopamine (PDA/PPY) was found; the resultant PDA/PPY films exhibited greatly increased adhesion strengths of up to 3.7 ± 0.8 MPa and the modified electrodes had electrochemical impedances two to three orders of magnitude lower than that of an unmodified electrode. This electrochemical deposition of adhesive and conductive PDA/PPY offers a facile and versatile electrode modification for various applications, such as biosensors and batteries. PMID:27459901

  2. Effects of electron-beam irradiation on conducting polypyrrole nanowires

    SciTech Connect

    Hong, Young Ki; Park, Dong Hyuk; Park, Se Hee; Park, Soung Kyu; Joo, Jinsoo

    2009-02-02

    Conducting polypyrrole (PPy) nanowires (NWs) were irradiated by a relatively high energy (300 keV-2 MeV) electron-beam (e-beam) generated from a linear electron accelerator in an atmospheric environment. From the current-voltage characteristics of pristine and 2 MeV e-beam irradiated PPy NWs, we observed a dramatic variation in resistance from 8.0x10{sup 2} to 1.45x10{sup 8} {omega}, that is, we observed a transition from conducting states to nonconducting states through the e-beam irradiation. To discern conformational changes and the doping states of PPy NWs through the e-beam irradiation, we measured Raman and ultraviolet-visible absorption spectra for the PPy NWs. As the energy of the e-beam irradiation increased, we observed that the PPy NWs were changed from doping states to dedoping states with conformational modification including the variation in {pi}-conjugation length.

  3. Effects of ultramicroelectrode dimensions on the electropolymerization of polypyrrole

    PubMed Central

    Fletcher, Benjamin L.; Fern, Jared T.; Rhodes, Kevin; McKnight, Timothy E.; Fowlkes, Jason D.; Retterer, Scott T.; Keffer, David J.; Simpson, Michael L.; Doktycz, Mitchel J.

    2009-01-01

    Anode geometry can significantly affect the electrochemical synthesis of conductive polymers. Here, the effects of anode dimensions on the electropolymerization of pyrrole are investigated. Band microelectrodes were prepared with widths ranging from 2 to 500 μm. The anode dimension has a significant effect on the resulting thickness of polymer film. The electropolymerization process deviates significantly from that predicted by simple mass transfer considerations when electrode dimensions are less than ∼20 μm. Polymer film thickness is thinner than expected when electrode dimensions become less than ∼10 μm. A simple mathematical model was derived to explain the observed effects of anode dimensions on the polymerization process. Simulation results confirm that diffusive loss of reaction intermediates accounts for the observed experimental trends. The described simulation facilitates understanding of the electropolymerization processes and approaches to the controlled deposition of polypyrrole, particularly at the submicron scale, for microelectromechanical systems and biomedical applications. PMID:19657404

  4. Corrosion behaviour of Nitinol alloy coated with alkylsilanes and polypyrrole.

    PubMed

    Flamini, D O; Saidman, S B

    2014-11-01

    Nitinol (equiatomic Ni and Ti alloy (NiTi)) substrate was modified using a coating system formed by a self-assembled film of alkylsilane compounds (propyltrichlorosilane (C3H7SiCl3) or octadecyltrichlorosilane (C18H37SiCl3)) and polypyrrole (PPy) doped with sodium bis(2-ethylhexyl) sulfosuccinate (Aerosol OT or AOT). The combination of alkylsilanes and the presence of a voluminous molecule like AOT entrapped into the PPy films improve the pitting corrosion resistance of the substrate in chloride solution. The best performance was achieved with the longest alkylsilane chains, where the PPy film remains adhered to the underlying coating after a pitting corrosion test. PMID:25280711

  5. ZnS-nanocrystals/polypyrrole nanocomposite film based immunosensor

    NASA Astrophysics Data System (ADS)

    Mishra, Sujeet K.; Pasricha, Renu; Biradar, Ashok M.; Rajesh

    2012-01-01

    We report an electrochemically synthesized ZnS nanocrystals modified polypyrrole (PPy) nanocomposite film based immunosensor for the detection of C-reactive protein (αCRP). The ZnS-PPy composite film was characterized by transmission electron microscopy (TEM), atomic force microscopy (AFM) and electrochemical techniques. The modified film showed good biocompatibility with efficient binding to protein antibody (αCRP-Ab) molecules through ZnS nanocrystals, exhibited an attractive platform for immunosensor fabrication. The electrical and sensing properties of the polymer composite film of different thickness towards protein antigen (αCRP-Ag) were delineated. The immunosensor exhibited an impedance response to αCRP-Ag concentration in a linear range from 10 ng to 10 μg mL-1.

  6. Characteristics of tantalum electrolytic capacitors using soluble polypyrrole electrolyte

    NASA Astrophysics Data System (ADS)

    Jang, Kwan Sik; Moon, Bongjin; Oh, Eung Ju; Lee, Hoosung

    Polypyrrole (Ppy) electrolyte solutions in various organic solvents (dimethylformamide, DMF; N-methyl-2-pyrrolidone, NMP; chloroform; trifluoroacetic acid) were prepared using Ppy powder doped with di(2-ethylhexyl)sulfosuccinate sodium salt (Ppy-DEHS) and butylnaphthalene sulfonate sodium salt (Ppy-BNS), respectively. Several tantalum electrolytic capacitors were fabricated by dip coating in these solutions and their electrical properties such as capacitance and tan δ were measured. The capacitors prepared with Ppy-DEHS electrolyte in trifluoroacetic acid showed both high capacitance and low tan δ. Usage of a Ppy electrolyte solution containing both surfactant and a coupling agent also resulted in high capacitance and low tan δ. These phenomena were interpreted in terms of electrical conductivity and chemical structure of the electrolyte, and interactions such as hydrogen bonding, radical addition reaction, covalent bonding between the tantalum oxide layer and the solvent.

  7. Electrochemical deposition of conductive and adhesive polypyrrole-dopamine films

    NASA Astrophysics Data System (ADS)

    Kim, Semin; Jang, Lindy K.; Park, Hyun S.; Lee, Jae Young

    2016-07-01

    Electrode surfaces have been widely modified with electrically conductive polymers, including polypyrrole (PPY), to improve the performance of electrodes. To utilize conductive polymers for electrode modification, strong adhesion between the polymer films and electrode substrates should be ensured with high electrical/electrochemical activities. In this study, PPY films were electrochemically polymerized on electrodes (e.g., indium tin oxide (ITO)) with dopamine as a bio-inspired adhesive molecule. Efficient and fast PPY electrodeposition with dopamine (PDA/PPY) was found; the resultant PDA/PPY films exhibited greatly increased adhesion strengths of up to 3.7 ± 0.8 MPa and the modified electrodes had electrochemical impedances two to three orders of magnitude lower than that of an unmodified electrode. This electrochemical deposition of adhesive and conductive PDA/PPY offers a facile and versatile electrode modification for various applications, such as biosensors and batteries.

  8. Ionic polymer metal composites with polypyrrole-silver electrodes

    NASA Astrophysics Data System (ADS)

    Cellini, F.; Grillo, A.; Porfiri, M.

    2015-03-01

    Ionic polymer metal composites (IPMCs) are a class of soft active materials that are finding increasing application in robotics, environmental sensing, and energy harvesting. In this letter, we demonstrate the fabrication of IPMCs via in-situ photoinduced polymerization of polypyrrole-silver electrodes on an ionomeric membrane. The composition, morphology, and sheet resistance of the electrodes are extensively characterized through a range of experimental techniques. We experimentally investigate IPMC electrochemistry through electrochemical impedance spectroscopy, and we propose a modified Randle's model to interpret the impedance spectrum. Finally, we demonstrate in-air dynamic actuation and sensing and assess IPMC performance against more established fabrication methods. Given the simplicity of the process and the short time required for the formation of the electrodes, we envision the application of our technique in the development of a rapid prototyping technology for IPMCs.

  9. On-chip metal/polypyrrole quasi-reference electrodes for robust ISFET operation.

    PubMed

    Duarte-Guevara, Carlos; Swaminathan, Vikhram V; Burgess, Mark; Reddy, Bobby; Salm, Eric; Liu, Yi-Shao; Rodriguez-Lopez, Joaquin; Bashir, Rashid

    2015-05-21

    To operate an ion-sensitive field-effect transistor (ISFETs) it is necessary to set the electrolyte potential using a reference electrode. Conventional reference electrodes are bulky, fragile, and too big for applications where the electrolyte volume is small. Several researchers have proposed tackling this issue using a solid-state planar micro-reference electrode or a reference field-effect transistor. However, these approaches are limited by poor robustness, high cost, or complex integration with other microfabrication processes. Here we report a simple method to create robust on-chip quasi-reference electrodes by electrodepositing polypyrrole on micro-patterned metal leads. The electrodes were fabricated through the polymerization of pyrrole on patterned metals with a cyclic voltammetry process. Open circuit potential measurements were performed to characterize the polypyrrole electrode performance, demonstrating good stability (±1 mV), low drift (∼1 mV h(-1)), and reduced pH response (5 mV per pH). In addition, the polypyrrole deposition was repeated in microelectrodes made of different metals to test compatibility with standard complementary metal-oxide-semiconductor (CMOS) processes. Our results suggest that nickel, a metal commonly used in semiconductor foundries for silicide formation, is a good candidate to form the polypyrrole quasi-reference electrodes. Finally, the polypyrrole microelectrodes were used to operate foundry fabricated ISFETs. These experiments demonstrated that transistors biased with polypyrrole electrodes have pH sensitivity and resolution comparable to ones that are biased with standard reference electrodes. Therefore, the simple fabrication, high compatibility, and robust electrical performance make polypyrrole an ideal choice for the fabrication of outstanding microreference electrodes that enable robust and sensitive operation of multiple ISFET sensors on a chip. PMID:25869990

  10. Synthesis and Microwave Absorption Properties of BaTiO3-polypyrrole Composite

    NASA Astrophysics Data System (ADS)

    Li, Qiao-ling; Zhang, Cun-rui; Li, Jian-qiang

    2010-10-01

    BaTiO3 powders are prepared by sol-gel method by cotton template. Polypyrrole is prepared by chemical oxidation route in the emulsion polymerization system. Then BaTiO3-polypyrrole composites with different mixture ratios are prepared by as-prepared material. The structure, morphology, and properties of the composites are characterized with Infrared spectrum, X-ray diffraction, scanning electron microscope, and net-wok analyzer. The complex permittivity and reflection loss of the composites are measured at different microwave frequencies in S-band and C-band (0.03-6 GHz) employing vector network analyzer model PNA 3629D vector. The effect of the mass ratio of BaTiO3 to polypyrrole on the microwave loss properties of the composites is investigated. A possible microwave absorbing mechanism of BaTiO3-polypyrrole composite is proposed. The BaTiO3-polypyrrole composite can find applications in suppression of electromagnetic interference and reduction of radar signature.

  11. Non-linear time variant model intended for polypyrrole-based actuators

    NASA Astrophysics Data System (ADS)

    Farajollahi, Meisam; Madden, John D. W.; Sassani, Farrokh

    2014-03-01

    Polypyrrole-based actuators are of interest due to their biocompatibility, low operation voltage and relatively high strain and force. Modeling and simulation are very important to predict the behaviour of each actuator. To develop an accurate model, we need to know the electro-chemo-mechanical specifications of the Polypyrrole. In this paper, the non-linear time-variant model of Polypyrrole film is derived and proposed using a combination of an RC transmission line model and a state space representation. The model incorporates the potential dependent ionic conductivity. A function of ionic conductivity of Polypyrrole vs. local charge is proposed and implemented in the non-linear model. Matching of the measured and simulated electrical response suggests that ionic conductivity of Polypyrrole decreases significantly at negative potential vs. silver/silver chloride and leads to reduced current in the cyclic voltammetry (CV) tests. The next stage is to relate the distributed charging of the polymer to actuation via the strain to charge ratio. Further work is also needed to identify ionic and electronic conductivities as well as capacitance as a function of oxidation state so that a fully predictive model can be created.

  12. Synthesis and Electrochemical Analysis of Algae Cellulose-Polypyrrole-Graphene Nanocomposite for Supercapacitor Electrode.

    PubMed

    Aphale, Ashish; Chattopadhyay, Aheli; Mahakalakar, Kapil; Patra, Prabir

    2015-08-01

    A novel nanocomposite has been developed using extracted cellulose from marine algae coated with conductive polypyrrole and graphene nanoplateletes. The nanocomposite fabricated via in situ polymerization was used as an electrode for a supercapacitor device. The nanocomposite material has been electrochemically characterized using cyclic voltammetry to test its potential to super-capacitive behavior. The specific capacitance of polypyrrole-graphene-cellulose nanocomposite as calculated from cyclic voltammetry curve is 91.5 Fg-1 at the scan rate 50 mV s-1. Transmission electron microscope images show the polymerized polypyrrole -graphene coated cellulosic nanofibers. Scanning electron microscope images reveal an interesting "necklace" like beaded morphology on the cellulose fibers. It is observed that the necklace like structure start to disintegrate with the increase in graphene concentration. The open circuit voltage of the device with polypyrrole-graphene-cellulose electrode was found to be around 225 mV and that of the polypyrrole-cellulose device is only 53 mV without graphene. The results suggest marked improvement in the performance of the nanocomposite supercapacitor device upon graphene inclusion. PMID:26369230

  13. New Secondary Batteries Utilizing Electronically Conductive Polypyrrole Cathode. Ph.D. Thesis

    NASA Technical Reports Server (NTRS)

    Yeu, Taewhan

    1991-01-01

    To gain a better understanding of the dynamic behavior in electronically conducting polypyrroles and to provide guidance toward designs of new secondary batteries based on these polymers, two mathematical models are developed; one for the potentiostatically controlled switching behavior of polypyrrole film, and one for the galvanostatically controlled charge/discharge behavior of lithium/polypyrrole secondary battery cell. The first model is used to predict the profiles of electrolyte concentrations, charge states, and electrochemical potentials within the thin polypyrrole film during switching process as functions of applied potential and position. Thus, the detailed mechanisms of charge transport and electrochemical reaction can be understood. Sensitivity analysis is performed for independent parameters, describing the physical and electrochemical characteristic of polypyrrole film, to verify their influences on the model performance. The values of independent parameters are estimated by comparing model predictions with experimental data obtained from identical conditions. The second model is used to predict the profiles of electrolyte concentrations, charge state, and electrochemical potentials within the battery system during charge and discharge processes as functions of time and position. Energy and power densities are estimated from model predictions and compared with existing battery systems. The independent design criteria on the charge and discharge performance of the cell are provided by studying the effects of design parameters.

  14. Bioelectrodes based on pseudocapacitive cellulose/polypyrrole composite improve performance of biofuel cell.

    PubMed

    Kizling, Michal; Stolarczyk, Krzysztof; Tammela, Petter; Wang, Zhaohui; Nyholm, Leif; Golimowski, Jerzy; Bilewicz, Renata

    2016-12-01

    Enzymatic electrodes with high internal capacitance, based on cellulose/polypyrrole composite were optimized and utilized to design improved enzymatic fuel cell. Fructose dehydrogenase Gluconobacter sp. specifically adsorbed on the cellulose/polypyrrole matrix and electrophoretically immobilized and electrochemically entrapped Laccase Trametes versicolor, were used as the anode and cathode bioelectrocatalysts, respectively. The cellulose/polypyrrole composite film exhibited pseudocapacitive properties under mild pH conditions. Following modification with carboxylic groups the composite material enabled highly efficient adsorption of enzyme and provided good electrical contact between the enzymatic active sites and the electrode surface. The modified cellulose/polypyrrole composite based electrode was used for the anode leading to mediatorless fructose oxidation giving large catalytic current density, 12.8mAcm(-2). Laccase and 2,2'-azino-bis(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) as the mediator entrapped in the cellulose/polypyrrole composite film generated dioxygen reduction current density of 2mAcm(-2). Application of pseudocapacitive matrix and decreasing the distance between electrodes to 1mm lead to improvement of the biofuel cell power output and its regeneration ability. The power of the cell was found to increase by introduction of a preconditioning step during which the cell was kept at open circuit voltage under fuel flow. After 24h of preconditioning the matrix was recharged and the device output reached the power, 2.1mWcm(-2) and OCV, 0.59V. PMID:26936112

  15. Optical properties of MgF2 nano-composite films dispersed with noble metal nanoparticles synthesized by sol-gel method

    NASA Astrophysics Data System (ADS)

    Wakaki, Moriaki; Soujima, Nobuaki; Shibuya, Takehisa

    2015-03-01

    Porous MgF2 films synthesized by a sol-gel method exhibit the lowest refractive index among the dielectric optical materials and are the most useful materials for the anti-reflection coatings. On the other hand, surface plasmon resonance (SPR) absorptions of noble metal nanoparticles in various solid matrices have been extensively studied. New functional materials like a SERS (Surface Enhanced Raman Spectroscopy) tips are expected by synthesizing composite materials between porous MgF2 films featured by the network of MgF2 nanoparticles and noble metal nanoparticles introduced within the network. In this study, fundamental physical properties including morphology and optical properties are characterized for these materials to make clear the potential of the composite system. Composite materials of MgF2 films dispersed with noble metal (Ag, Au) nanoparticles were prepared using the sol-gel technique with various annealing temperatures and densities of noble metal nanoparticles. The structural morphology was analyzed by an X-ray diffractometer (XRD) and a scanning electron microscope (SEM). The size and shape distributions of the metal nanoparticles were observed using a transmission electron microscope (TEM). The optical properties of fabricated composite films were characterized by UV-Vis-NIR and FT-IR spectrophotometers. The absorption spectra due to the surface plasmon resonance (SPR) of the metal nanoparticles were analyzed using the dielectric function considering the effective medium approximation, typically Maxwell-Garnett model. The Raman scattering spectra were also studied to check the enhancement effect of specimen dropped on the MgF2: Ag nano-composite films deposited on Si substrate. Enhancement of the Raman intensity of pyridine solution specimen was observed.

  16. Development of TiO2-Xwt%InVO4 Photocatalytic Nano-composites for Ambient Light Assisted Water Detoxification

    NASA Astrophysics Data System (ADS)

    Srinivasan, Sesha; Wilson, Jeremiah; Vickers, Eric; Integlia, Ryan

    2015-03-01

    We have developed nano-composites of TiO2-Xwt%InVO4 for environmental and biomedical research applications. TiO2 is commonly used as catalyst that utilizes the UV portion of the sun light spectrum to induce photo-oxidation and photo-reduction processes. We hypothesized that the combination of InVO4 and TiO2 will result in a material that will catalyze organic contaminants through photo-oxidation under visible light. We combined TiO2 with 2,4,6,8,10wt% of InVO4 via wet ball milling process. We have compared the various concentrations of InVO4 on TiO2 matrix by SEM, BET surface area analyzer, FTIR, XRD, and photodegradation of the organic contaminant Methyl Orange. After characterization we found that 4wt% InVO4 + TiO2 mixture displayed the most promising characteristics for photo-oxidation under visible light; From the BET surface area analysis it showed the largest surface area out of the prior mentioned TiO2 = Xwt% InVO4 mixtures and a degradation amount equivalent to 50% of Methyl Orange contaminant over 7 hours under visible light. In conclusion, TiO2-Xwt%InVO4 displayed evidence of photo-oxidation under visible light conditions. Authors would like to acknowledge the support from Sigma Pi Sigma and Society of Physics Students. National Science Foundation and Florida Energy Systems Consortium are gratefully acknowledged for the research and education grants.

  17. In vitro biocompatibility of polypyrrole/PLGA conductive nanofiber scaffold with cultured rat hepatocytes

    NASA Astrophysics Data System (ADS)

    Chu, Xue-Hui; Xu, Qian; Feng, Zhang-Qi; Xiao, Jiang-Qiang; Li, Qiang; Sun, Xi-Tai; Cao, Yang; Ding, Yi-Tao

    2014-09-01

    To intruduce conductive biomaterial into liver tissue engineering, a conductive nanofiber scaffold, polypyrrole/poly(lactic-co-glycolic)acid(PLGA), was designed and prepared via electro-spinning and oxidative polymerization. Effects of the scaffold on hepatocyte adhesion, viability and function were then investigated. SEM revealed pseudopodium formation and abundant extracellular matrix on the surface of PLGA membrane and polypyrrole/PLGA membrane. The adhesion rate, cellular activity, urea synthesis and albumin secretion of the hepatocytes cultured on polypyrrole/PLGA group were similar to those on the PLGA group, but were significantly higher than those on the control group. There were no significant differences in concentrations of LDH and TNF-α among three groups. These results suggested the potential application of this conductive nanofiber scaffold as a suitable substratum for hepatocyte culturing in liver tissue engineering.

  18. Nanostructured polypyrrole/carbon composite as Pt catalyst support for fuel cell applications

    NASA Astrophysics Data System (ADS)

    Zhao, Hongbin; Li, Lei; Yang, Jun; Zhang, Yongming

    A novel catalyst support was synthesized by in situ chemical oxidative polymerization of pyrrole on Vulcan XC-72 carbon in naphthalene sulfonic acid (NSA) solution containing ammonium persulfate as oxidant at room temperature. Pt nanoparticles with 3-4 nm size were deposited on the prepared polypyrrole-carbon composites by chemical reduction method. Scanning electron microscopy and transmission electron microscopy measurements showed that Pt particles were homogeneously dispersed in polypyrrole-carbon composites. The Pt nanoparticles-dispersed catalyst composites were used as anodes of fuel cells for hydrogen and methanol oxidation. Cyclic voltammetry measurements of hydrogen and methanol oxidation showed that Pt nanoparticles deposited on polypyrrole-carbon with NSA as dopant exhibit better catalytic activity than those on plain carbon. This result might be due to the higher electrochemically available surface areas, electronic conductivity and easier charge-transfer at polymer/carbon particle interfaces allowing a high dispersion and utilization of deposited Pt nanoparticles.

  19. One-step synthesis of branched sulfur/polypyrrole nanocomposite cathode for lithium rechargeable batteries

    NASA Astrophysics Data System (ADS)

    Zhang, Yongguang; Bakenov, Zhumabay; Zhao, Yan; Konarov, Aishuak; Doan, The Nam Long; Malik, Muhammad; Paron, Todd; Chen, P.

    2012-06-01

    A nanostructured sulfur/polypyrrole binary composite was prepared by a simple one-step ballmilling without heat-treatment. High resolution transmission and scanning electronic microscopy showed the formation of a highly developed branched structure consisting of polypyrrole with uniform sulfur coating on its surface. Exclusion of heat-treatment in the composite preparation avoided the sulfur loss; the composite contained 65 wt% of sulfur. AC impedance spectroscopy data exhibited remarkable reduction in charge transfer resistance of the composite compared with pristine sulfur. This may be due to the high conductivity and large surface area of polypyrrole. This charge transfer enhancement led to the electrochemical performance improvement of the composite cathode, delivering first discharge capacity of 1320 mAh g-1.

  20. Template electropolymerization of polypyrrole nanostructures on highly ordered pyrolytic graphite step and pit defects

    SciTech Connect

    Noll, J.D.; Nicholson, M.A.; Myrick, M.L.; Van Patten, P.G.; Chung, C.W.

    1998-10-01

    Polypyrrole nanostructures with diameters {le}10 nm have been electropolymerized using step and pit defects on highly ordered pyrolytic graphite (HOPG) as templates for electropolymerization. Step defects were naturally occurring, and pits were formed via oxidation of freshly cleaved surfaces of an HOPG water by heating at {approximately}640 C. Underpotential deposition of {approximately}80 mV caused polypyrrole to form only on the step and pit edges of HOPG at and not on the basal plane. The size of these nanostructures could be controlled by limiting the pyrrole polymerization time at anodic potentials. Recent modeling results allow the morphology of the deposition to be inferred, and the authors find the electrochemical data consistent with wire-shaped growth for up to 30 s at constant potential, after which the growth changes morphology. Scanning tunneling microscopy data confirm this result. Preliminary studies show that these polypyrrole nanostructures can be removed by sonication.

  1. Improvement of lithium storage performance of Sn-alloy anode materials by a polypyrrole protective layer

    NASA Astrophysics Data System (ADS)

    Peng, Peng; Wen, Zhaoyin; Liu, Yu; Jin, Jun

    2015-01-01

    The SnO2-based anode with improved reversible capacity and cyclability was achieved by employing a protective layer composed of crosslinked polypyrrole nanowires. Scanning electron microscopy measurement was performed to characterize the surface and cross section morphology of electrodes before and after cycling. The crosslinked polypyrrole nanowire protective layer with good elasticity adhered to the SnO2 surface could form a network, leading to buffer the volumetric swelling of active materials during the lithiation/delithiation process. A good cycling stability and an excellent rate capability of the modified electrode were achieved.

  2. Fabrication of a polymer battery based on polypyrrole electrodes and a polymer gel electrolyte

    SciTech Connect

    Killian, J.G.; Coffey, B.M.; Poehler, T.O.; Searson, P.C.

    1995-12-31

    The electronic conductivity and redox behavior of conjugated polymers make them suitable for charge storage applications. The authors present preliminary results for an all polymer system consisting of a p-doped polypyrrole cathode and pseudo n-doped polypyrrole/polystyrenesulfonate anode. Using a thin film construction technique, electrodes were assembled into cells using a polymer gel electrolyte based on polyacrylonitrile, which has a high room temperature conductivity. Charge capacities of 13 mAh g{sup {minus}1} based on the mass of the electroactive polymer in the cathode have been obtained for over 100 cycles.

  3. Enhanced electrochromic properties of a polypyrrole-indigo carmine-gold nanoparticles nanocomposite.

    PubMed

    Loguercio, L F; Alves, C C; Thesing, A; Ferreira, J

    2015-01-14

    An indigo carmine doped polypyrrole embedded with gold nanoparticles nanocomposite (PPy-IC-Aunanop) was synthesized by in situ electrochemical polymerization of polypyrrole in the presence of HAuCl4. The nanocomposite was characterized by in situ spectroelectrochemical experiments to study the effect of embedded gold nanoparticles on the electrochromic properties of the material. The results show the formation of a nanocomposite presenting enhanced electrochromic and optical properties, higher electroactivity and 10% lower band-gap energies. The PPy-IC-Aunanop presented a two-fold increase in optical contrast when compared to PPy-IC, in addition to better optical stability. PMID:25418577

  4. Flexible strain sensor for air muscles using polypyrrole coated rubber

    NASA Astrophysics Data System (ADS)

    Tjahyono, Arief P.; Aw, Kean C.; Travas-Sejdic, Jadranka; Li, K. C.

    2010-04-01

    A novel flexible large strain sensor was developed to be use with an air muscle. A piece of butyl rubber was coated with the conducting polymer, polypyrrole through bulk solution and chemical vapour deposition method. The strain sensor was able to response to sudden movements represented by the multiple step functions of the applied strain. Consistency of the sensor's output was studied and the average error in the change of resistance was calculated to be 0.32% and 0.72% for elongation and contraction respectively for the sample made using chemical vapour deposition. However, a hysteresis was observed for this sample for a single cycle of elongation and contraction with the highest error calculated to be 3.2% at a 0% applied strain. SEM images showed the propagation of surface micro-cracks as the cause of the variation in surface resistance with applied strain. In addition, slower relaxation rate of the rubber prevented the surface micro-cracks to open and close at the same rate. The idea of utilizing conducting polymer coating can be applied to the inner rubber tube of the air muscle. As such, a complete integration between actuator and sensor can be realized.

  5. Electropolymerized molecularly imprinted polypyrrole film for sensing of clofibric acid.

    PubMed

    Schweiger, Bianca; Kim, Jungtae; Kim, Young Jun; Ulbricht, Mathias

    2015-01-01

    Piezoelectric quartz crystals and analogous gold substrates were electrochemically coated with molecularly imprinted polypyrrole films for pulsed amperometric detection (PAD) of clofibric acid, a metabolite of clofibrate. Cyclic voltammetry data obtained during polymerization and deposited weight estimations revealed a decrease of the polymerization rate with increasing clofibric acid concentration. XPS measurements indicated that clofibric acid could be removed after imprinting with an aqueous ethanol solution, which was further optimized by using PAD. Zeta potential and contact angle measurements revealed differences between molecularly imprinted (MIP) and non-imprinted polymer (NIP) layers. Binding experiments with clofibric acid and other substances showed a pronounced selectivity of the MIP for clofibric acid vs. carbamazepine, but the response of MIP and NIP to 2,4-dichlorophenoxyacetic acid was higher than that for clofibric acid. A smooth surface, revealed by AFM measurements, with roughness of 6-8 nm for imprinted and non-imprinted layers, might be a reason for an excessively low density of specific binding sites for clofibric acid. Furthermore, the decreased polymerization rate in the presence of clofibric acid might not result in well-defined polymer structures, which could be the reason for the lower sensitivity. PMID:25730487

  6. Investigation of polypyrrole degradation using electrochemical impedance spectroscopy.

    PubMed

    Marchesi, L F Q P; Simões, F R; Pocrifka, L A; Pereira, E C

    2011-08-11

    In this paper, the electrochemical degradation of polypyrrole film was studied by means of overpotential application. The overpotential was 0.58 V versus SCE, and after every 5 min of application of 0.58 V, a cyclic voltammogram was recorded in the range of -0.7 to 0.5 V as well as an electrochemical impedance spectroscopy and electrochemical quartz crystal microbalance (EIS and EQCM). The main characteristic is the huge increase in the charge transfer resistance (r(ct)), which indicates that the insertion process of ions in the polymer matrix is hindered by the electrochemical degradation. Once the process of insertion is damaged, the number of intercalated ions in the matrix should decrease, which is expressed by the low-frequency capacitance, which is proportional to the number of intercalated ions in the polymeric matrix. The decrease of intercalated ions has an influence in the mass variation of the polymer film, which is confirmed by EQCM measurements. PMID:21721565

  7. Biocompatible xanthan/polypyrrole scaffolds for tissue engineering.

    PubMed

    Bueno, Vania Blasques; Takahashi, Suelen Harumi; Catalani, Luiz Henrique; de Torresi, Susana Ines Cordoba; Petri, Denise Freitas Siqueira

    2015-01-01

    Polypyrrole (PPy) was electropolymerized in xanthan hydrogels (XCA), resulting in electroactive XCAPPy scaffolds with (15 ± 3) wt.% PPy and (40 ± 10) μm thick. The physicochemical characterization of hybrid XCAPPy scaffolds was performed by means of cyclic voltammetry, swelling tests, Fourier transform infrared spectroscopy (FTIR), differential scanning calorimetry (DSC), thermogravimetric analyses (TGA), scanning electron microscopy (SEM), atomic force microscopy (AFM) and tensile tests. XCAPPy swelled~80% less than XCA. FTIR spectra and thermal analyses did not evidence strong interaction between PPy and XCA matrix. XCAPPy presented a porous stratified structure resulting from the arrangement of PPy chains parallel to XCA surface. Under stress XCAPPy presented larger strain than neat XCA probably due to the sliding of planar PPy chains. The adhesion and proliferation of fibroblasts onto XCA and XCAPPy were evaluated in the absence and in the presence of external magnetic field (EMF) of 0.4T, after one day, 7 days, 14 days and 21 days. Fibroblast proliferation was more pronounced onto XCAPPy than onto XCA, due to its higher hydrophobicity and surface roughness. EMF stimulated cell proliferation onto both scaffolds. PMID:25953548

  8. Electropolymerized Molecularly Imprinted Polypyrrole Film for Sensing of Clofibric Acid

    PubMed Central

    Schweiger, Bianca; Kim, Jungtae; Kim, Young Jun; Ulbricht, Mathias

    2015-01-01

    Piezoelectric quartz crystals and analogous gold substrates were electrochemically coated with molecularly imprinted polypyrrole films for pulsed amperometric detection (PAD) of clofibric acid, a metabolite of clofibrate. Cyclic voltammetry data obtained during polymerization and deposited weight estimations revealed a decrease of the polymerization rate with increasing clofibric acid concentration. XPS measurements indicated that clofibric acid could be removed after imprinting with an aqueous ethanol solution, which was further optimized by using PAD. Zeta potential and contact angle measurements revealed differences between molecularly imprinted (MIP) and non-imprinted polymer (NIP) layers. Binding experiments with clofibric acid and other substances showed a pronounced selectivity of the MIP for clofibric acid vs. carbamazepine, but the response of MIP and NIP to 2,4-dichlorophenoxyacetic acid was higher than that for clofibric acid. A smooth surface, revealed by AFM measurements, with roughness of 6–8 nm for imprinted and non-imprinted layers, might be a reason for an excessively low density of specific binding sites for clofibric acid. Furthermore, the decreased polymerization rate in the presence of clofibric acid might not result in well-defined polymer structures, which could be the reason for the lower sensitivity. PMID:25730487

  9. Polypyrrole electrodes doped with sulfanilic acid azochromotrop for electrochemical supercapacitors

    NASA Astrophysics Data System (ADS)

    Chen, S.; Zhitomirsky, I.

    2013-12-01

    In this work we demonstrate the feasibility of deposition of polypyrrole (PPy) films by electropolymerization on stainless steel substrates and fabrication of PPy powders by chemical polymerization using sulfanilic acid azochromotrop (SPADNS) as a new anionic dopant. The problem of low adhesion of PPy films to stainless steel substrates is addressed by the use of SPADNS, which exhibits chelating properties, promoting film formation. The use of fine particles, prepared by the chemical polymerization method, allows impregnation of Ni foams and fabrication of porous electrodes with high materials loading for electrochemical supercapacitors (ES). PPy films and Ni foam based PPy electrodes show capacitive behaviour in Na2SO4 electrolyte. The electron microscopy studies, impedance spectroscopy data and analysis of the SPADNS structure provide an insight into the factors, controlling capacitive behaviour. The Ni foam based electrodes offer advantages of improved capacitive behaviour at high materials loadings and good cycling stability. The area normalized and volume normalized specific capacitances are as high as 5.43 F cm-2 and 93.6 F cm-3, respectively, for materials loading of 35.4 mg cm-2. The capacitance retention of Ni foam based electrodes is 91.5% after 1000 cycles. The Ni foam based PPy electrodes are promising for application in ES.

  10. Labeled magnetic nanoparticles assembly on polypyrrole film for biosensor applications.

    PubMed

    Fredj, H Ben; Helali, S; Esseghaier, C; Vonna, L; Vidal, L; Abdelghani, A

    2008-05-15

    In recent years, conducting polymers combined with metallic nanoparticles have been paid more attention due to their potential applications in microelectronics, microsystems, optical sensors and photoelectronic chemistry. The work presented in this paper describes the preparation and characterization of a nanocomposite composed by a thin polypyrrole (PPy) film covered with an assembly of magnetic nanoparticles (NPs). The magnetic particles were immobilized on PPy films under appropriate magnetic field in order to control their organization on the PPy film and finally to improve the sensitivity of the system in potential sensing applications. The electrical properties and morphology of the resulting PPy film and the PPy film/NPs composite were characterized with cyclic voltammetry, impedance spectroscopy (IS), scanning electron microscopy (SEM), atomic force microscopy (AFM) and infra-red spectroscopy (IR). By using streptavidin labeled magnetic particles it was possible to functionalize the NPs assembly with biotin-Fab fragment K47 antibody. The designed biosensor had been successfully applied in rapid, simple, and accurate measurements of atrazine concentrations, with a significantly low detection limit of 5 ng/ml. PMID:18585140

  11. Hierarchical polypyrrole based composites for high performance asymmetric supercapacitors

    NASA Astrophysics Data System (ADS)

    Chen, Gao-Feng; Liu, Zhao-Qing; Lin, Jia-Ming; Li, Nan; Su, Yu-Zhi

    2015-06-01

    An advanced asymmetric supercapacitor with high energy density, exploiting hierarchical polypyrrole (PPy) based composites as both the anode [three dimensional (3D) chuzzle-like Ni@PPy@MnO2] and (3D cochleate-like Ni@MnO2@PPy) cathode, has been developed. The ultrathin PPy and flower-like MnO2 orderly coating on the high-conductivity 3D-Ni enhance charge storage while the unique 3D chuzzle-like and 3D cochleate-like structures provide storage chambers and fast ion transport pathways for benefiting the transport of electrolyte ions. The 3D cochleate-like Ni@MnO2@PPy possesses excellent pseudocapacitance with a relatively negative voltage window while preserved EDLC and free transmission channels conducive to hold the high power, providing an ideal cathode for the asymmetric supercapacitor. It is the first report of assembling hierarchical PPy based composites as both the anode and cathode for asymmetric supercapacitor, which exhibits wide operation voltage of 1.3-1.5 V with maximum energy and power densities of 59.8 Wh kg-1 and 7500 W kg-1.

  12. Dynamic mechanoelectrochemistry of polypyrrole membranes via shear-force tracking.

    PubMed

    Northcutt, Robert G; Heinemann, Christian; Sundaresan, Vishnu Baba

    2016-07-14

    Mechanoelectrochemistry is the study of elastic and plastic deformation of materials during reversible reduction and oxidation processes. In this article, we introduce shear-force tracking as a method to dynamically measure mechanical (strain), chemical (ion transport), and electrical (applied redox potentials) responses of the conducting polymer polypyrrole (PPy) during redox reactions. This tracking technique uses a control algorithm to maintain a set distance between a ultramicroelectrode (UME) tip and a surface via shear-force regulation. Due to the sensitivity of shear-force signals in the near field of substrate surfaces, a significantly improved signal to noise ratio (20 : 1) is possible and allows for nanoscale measurement of redox events. Chemomechanical coupling (the ratio of ion transport to resultant extensional actuation) is calculated for PPy-based membranes of various thicknesses based on a mechanistic interpretation of charge storage in redox active conducting polymers. The measured dynamic response demonstrates that chemomechanical coupling is not a constant, as assumed in literature, but is dependent on the polymers state of charge and the direction (ingress/egress) of ion transport. PMID:27263628

  13. Mössbauer spectroscopy studies of selected conducting polypyrroles

    NASA Astrophysics Data System (ADS)

    Proń, A.; Kucharski, Z.; Budrowski, C.; Zagórska, M.; Krichene, S.; Suwalski, J.; Dehe, G.; Lefrant, S.

    1985-12-01

    Polypyrrole obtained by chemical oxidation of pyrrole in ethanol-water solution containing FeCl3 can be reduced chemically in Na+Naph-/THF solution and then reoxidized with FeCl3, SnCl4, and SbCl5. 57Fe and 119Sn Mössbauer spectra of the reaction products show only one type of iron and tin with Mössbauer parameters characteristic of FeCl-4 and SnCl-5. In the case of the oxidation with SbCl5, two nonequivalent antimony nuclei have been detected by 121Sb. The calculated isomer shift and quadrupole splitting values are consistent with SbCl-6 and SbCl3. The resonant absorption in all three systems studied is strongly temperature dependent and can be observed only at temperatures significantly lower than RT. This behavior indicates a low Mössbauer lattice temperature and an extremely loose bonding between the inserted anions and polymer chains.

  14. A Combined Molecular Dynamics and Experimental Study of Doped Polypyrrole.

    PubMed

    Fonner, John M; Schmidt, Christine E; Ren, Pengyu

    2010-10-01

    Polypyrrole (PPy) is a biocompatible, electrically conductive polymer that has great potential for battery, sensor, and neural implant applications. Its amorphous structure and insolubility, however, limit the experimental techniques available to study its structure and properties at the atomic level. Previous theoretical studies of PPy in bulk are also scarce. Using ab initio calculations, we have constructed a molecular mechanics force field of chloride-doped PPy (PPyCl) and undoped PPy. This model has been designed to integrate into the OPLS force field, and parameters are available for the Gromacs and TINKER software packages. Molecular dynamics (MD) simulations of bulk PPy and PPyCl have been performed using this force field, and the effects of chain packing and electrostatic scaling on the bulk polymer density have been investigated. The density of flotation of PPyCl films has been measured experimentally. Amorphous X-ray diffraction of PPyCl was obtained and correlated with atomic structures sampled from MD simulations. The force field reported here is foundational for bridging the gap between experimental measurements and theoretical calculations for PPy based materials. PMID:21052521

  15. A Combined Molecular Dynamics and Experimental Study of Doped Polypyrrole

    PubMed Central

    Fonner, John M.; Schmidt, Christine E.; Ren, Pengyu

    2010-01-01

    Polypyrrole (PPy) is a biocompatible, electrically conductive polymer that has great potential for battery, sensor, and neural implant applications. Its amorphous structure and insolubility, however, limit the experimental techniques available to study its structure and properties at the atomic level. Previous theoretical studies of PPy in bulk are also scarce. Using ab initio calculations, we have constructed a molecular mechanics force field of chloride-doped PPy (PPyCl) and undoped PPy. This model has been designed to integrate into the OPLS force field, and parameters are available for the Gromacs and TINKER software packages. Molecular dynamics (MD) simulations of bulk PPy and PPyCl have been performed using this force field, and the effects of chain packing and electrostatic scaling on the bulk polymer density have been investigated. The density of flotation of PPyCl films has been measured experimentally. Amorphous X-ray diffraction of PPyCl was obtained and correlated with atomic structures sampled from MD simulations. The force field reported here is foundational for bridging the gap between experimental measurements and theoretical calculations for PPy based materials. PMID:21052521

  16. The application of polypyrrole trilayer actuators in microfluidics and robotics

    NASA Astrophysics Data System (ADS)

    Kiefer, Rudolf; Mandviwalla, Xerxes; Archer, Rosalind; Tjahyono, Sungkono Surya; Wang, Han; MacDonald, Bruce; Bowmaker, Graham A.; Kilmartin, Paul A.; Travas-Sejdic, Jadranka

    2008-03-01

    Trilayer actuators were constructed using polypyrrole (PPy) films doped with dodecylbenzene sulfonate (DBS). Identical 5-20 μm PPy/DBS films were grown on either side of a 110 μm poly(vinylidene fluoride) (PVDF) membrane to serve as working and counter electrodes with respect to each other. The performance of the trilayer actuator was tested using potential step experiments between -0.8 and +0.8 V at different frequencies (0.03 to 10 Hz) and trilayer lengths (1 to 2.5 cm), and the extent of deflection was measured using a CCD camera. Satisfactory deflections in the range of 1-3 mm were observed for 10 μm thick PPy layers on trilayers 1.5 to 2.5 cm in length when operated at 1-5 Hz for over 40,000 cycles. The trilayer actuators were examined in a fluidics channels, and mathematical modelling using finite element analysis was used to predict overall fluid movement and flow rates. The trilayers were also used to construct a 'fish-tail' positioned at the back of a self-driven robotic fish.

  17. Transparent conductive nano-composites

    DOEpatents

    Geohegan, David Bruce; Ivanov, Ilia N.; Puretzky, Alexander A.; Jesse, Stephen; Hu, Bin; Garrett, Matthew; Zhao, Bin

    2011-04-12

    The present invention, in one embodiment, provides a method of forming an organic electric device that includes providing a plurality of carbon nanostructures; and dispersing the plurality of carbon nanostructures in a polymeric matrix to provide a polymeric composite, wherein when the plurality of carbon nanostructures are present at a first concentration an interface of the plurality of carbon nanostructures and the polymeric matrix is characterized by charge transport when an external energy is applied, and when the plurality of carbon nanostructures are present at a second concentration the interface of the plurality of carbon nanostructures and the polymeric matrix are characterized by exciton dissociation when an external energy is applied, wherein the first concentration is less than the second concentration.

  18. Transparent conductive nano-composites

    DOEpatents

    Geohegan, David Bruce; Ivanov, Ilia N; Puretzky, Alexander A; Jesse, Stephen; Hu, Bin; Garrett, Matthew; Zhao, Bin

    2013-09-24

    The present invention, in one embodiment, provides a method of forming an organic electric device that includes providing a plurality of carbon nanostructures; and dispersing the plurality of carbon nanostructures in a polymeric matrix to provide a polymeric composite, wherein when the plurality of carbon nanostructures are present at a first concentration an interface of the plurality of carbon nanostructures and the polymeric matrix is characterized by charge transport when an external energy is applied, and when the plurality of carbon nanostructures are present at a second concentration the interface of the plurality of carbon nanostructures and the polymeric matrix are characterized by exciton dissociation when an external energy is applied, wherein the first concentration is less than the second concentration.

  19. Nano-composite stainless steel

    DOEpatents

    Dehoff, Ryan R.; Blue, Craig A.; Peter, William H.; Chen, Wei; Aprigliano, Louis F.

    2015-07-14

    A composite stainless steel composition is composed essentially of, in terms of wt. % ranges: 25 to 28 Cr; 11 to 13 Ni; 7 to 8 W; 3.5 to 4 Mo; 3 to 3.5 B; 2 to 2.5 Mn; 1 to 1.5 Si; 0.3 to 1.7 C; up to 2 O; balance Fe. The composition has an austenitic matrix phase and a particulate, crystalline dispersed phase.

  20. Dual delivery of BMP-2 and bFGF from a new nano-composite scaffold, loaded with vascular stents for large-size mandibular defect regeneration.

    PubMed

    Su, Jiansheng; Xu, Hongzhen; Sun, Jun; Gong, Xue; Zhao, Hang

    2013-01-01

    The aim of this study was to investigate the feasibility and advantages of the dual delivery of bone morphogenetic protein-2 (BMP-2) and basic fibroblast growth factor (bFGF) from nano-composite scaffolds (PLGA/PCL/nHA) loaded with vascular stents (PLCL/Col/nHA) for large bone defect regeneration in rabbit mandibles. Thirty-six large bone defects were repaired in rabbits using engineering bone composed of allogeneic bone marrow mesenchymal stem cells (BMSCs), bFGF, BMP-2 and scaffolds composed of PLGA/PCL/nHA loaded with PLCL/Col/nHA. The experiments were divided into six groups: BMSCs/bFGF/BMP-2/scaffold, BMSCs/BMP-2/scaffold, BMSCs/bFGF/scaffold, BMSCs/scaffold, scaffold alone and no treatment. Sodium alginate hydrogel was used as the carrier for BMP-2 and bFGF and its features, including gelling, degradation and controlled release properties, was detected by the determination of gelation and degradation time coupled with a controlled release study of bovine serum albumin (BSA). AlamarBlue assay and alkaline phosphatase (ALP) activity were used to evaluate the proliferation and osteogenic differentiation of BMSCs in different groups. X-ray and histological examinations of the samples were performed after 4 and 12 weeks post-implantation to clarify new bone formation in the mandible defects. The results verified that the use of sodium alginate hydrogel as a controlled release carrier has good sustained release ability, and the combined application of bFGF and BMP-2 could significantly promote the proliferation and osteogenic differentiation of BMSCs (p < 0.05 or p < 0.01). In addition, X-ray and histological examinations of the samples exhibited that the dual release group had significantly higher bone formation than the other groups. The above results indicate that the delivery of both growth factors could enhance new bone formation and vascularization compared with delivery of BMP-2 or bFGF alone, and may supply a promising way of repairing large bone defects in