Science.gov

Sample records for nano-composite cation-exchanger polypyrrole

  1. 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

    2015-12-04

    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.

  2. 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.

  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. Forging Colloidal Nanostructures via Cation Exchange Reactions

    PubMed Central

    2016-01-01

    Among the various postsynthesis treatments of colloidal nanocrystals that have been developed to date, transformations by cation exchange have recently emerged as an extremely versatile tool that has given access to a wide variety of materials and nanostructures. One notable example in this direction is represented by partial cation exchange, by which preformed nanocrystals can be either transformed to alloy nanocrystals or to various types of nanoheterostructures possessing core/shell, segmented, or striped architectures. In this review, we provide an up to date overview of the complex colloidal nanostructures that could be prepared so far by cation exchange. At the same time, the review gives an account of the fundamental thermodynamic and kinetic parameters governing these types of reactions, as they are currently understood, and outlines the main open issues and possible future developments in the field. PMID:26891471

  5. Cation exchange capacity of pine bark substrates

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Cation exchange capacity (CEC) is an important soil and substrate chemical property. It describes a substrate's ability to retain cation nutrients. Higher CEC values for a substrate generally result in greater amounts of nutrients retained in the substrate and available for plant uptake, and great...

  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. Nanoheterostructure cation exchange: anionic framework conservation.

    PubMed

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

    2010-07-28

    In ionic nanocrystals the cationic sublattice can be replaced with a different metal ion via a fast, simple, and reversible place exchange, allowing postsynthetic modification of the composition of the nanocrystal, while preserving its size and shape. Here, we demonstrate 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 Cu(2)Se/Cu(2)S 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.

  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

    2015-02-03

    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.

  11. Cation-exchange chromatography of monoclonal antibodies

    PubMed Central

    Urmann, Marina; Graalfs, Heiner; Joehnck, Matthias; Jacob, Lothar R

    2010-01-01

    A novel cation-exchange resin, Eshmuno™ S, was compared to Fractogel® SO3− (M) and Toyopearl GigaCap S-650M. The stationary phases have different base matrices and carry specific types of polymeric surface modifications. Three monoclonal antibodies (mAbs) were used as model proteins to characterize these chromatographic resins. Results from gradient elutions, stirred batch adsorptions and confocal laser scanning microscopic investigations were used to elucidate binding behavior of mAbs onto Eshmuno™ S and Fractogel® SO3− and the corresponding transport mechanisms on these two resins. The number of charges involved in mAb binding for Eshmuno™ S is lower than for Fractogel® SO3−, indicating a slightly weaker electrostatic interaction. Kinetics from batch uptake experiments are compared to kinetic data obtained from confocal laser scanning microscopy images. Both experimental approaches show an accelerated protein adsorption for the novel stationary phase. The influence of pH, salt concentrations and residence times on dynamic binding capacities was determined. A higher dynamic binding capacity for Eshmuno™ S over a wider range of pH values and residence times was found compared to Fractogel® SO3− and Toyopearl GigaCap S-650M. The capture of antibodies from cell culture supernatant, as well as post-protein A eluates, were analyzed with respect to their host cell protein (hcp) removal capabilities. Comparable or even better hcp clearance was observed at much higher protein loading for Eshmuno™ S than Fractogel® SO3− or Toyopearl GigaCap S-650M. PMID:20559022

  12. Synthesis of Silver Embedded Poly(o-Anisidine) Molybdophosphate Nano Hybrid Cation-Exchanger Applicable for Membrane Electrode

    PubMed Central

    Khan, Anish; Khan, Aftab Aslam Parwaz; Asiri, Abdullah M.; Rub, Malik Abdul

    2014-01-01

    Poly(o-anisidine) molybdophosphate was expediently obtained by sol-gel mixing of Poly(o-anisidine) into the inorganic matrices of molybdophosphate, which was allowed to react with silver nitrate to the formation of poly(o-anisidine) molybdophosphate embedded silver nano composite. The composite was characterized by Fourier Transform Infrared Spectroscopy, X-ray powder diffraction, UV-Vis Spectrophotometry, Fluorescence Spectroscopy, Scanning Electron Microscopy/Energy-dispersive X-ray Spectroscopy and Thermogravimertic Analysis. Ion exchange capacity and distribution studies were carried out to understand the ion-exchange capabilities of the nano composite. On the basis of highest distribution studies, this nano composite cation exchanger was used as preparation of heavy metal ion selective membrane. Membrane was characterized for its performance as porosity and swelling later on was used for the preparation of membrane electrode for Hg(II), having better linear range, wide working pH range (2–4.5) with fast response in the real environment. PMID:24805257

  13. Synthesis of silver embedded poly(o-anisidine) molybdophosphate nano hybrid cation-exchanger applicable for membrane electrode.

    PubMed

    Khan, Anish; Khan, Aftab Aslam Parwaz; Asiri, Abdullah M; Rub, Malik Abdul

    2014-01-01

    Poly(o-anisidine) molybdophosphate was expediently obtained by sol-gel mixing of Poly(o-anisidine) into the inorganic matrices of molybdophosphate, which was allowed to react with silver nitrate to the formation of poly(o-anisidine) molybdophosphate embedded silver nano composite. The composite was characterized by Fourier Transform Infrared Spectroscopy, X-ray powder diffraction, UV-Vis Spectrophotometry, Fluorescence Spectroscopy, Scanning Electron Microscopy/Energy-dispersive X-ray Spectroscopy and Thermogravimertic Analysis. Ion exchange capacity and distribution studies were carried out to understand the ion-exchange capabilities of the nano composite. On the basis of highest distribution studies, this nano composite cation exchanger was used as preparation of heavy metal ion selective membrane. Membrane was characterized for its performance as porosity and swelling later on was used for the preparation of membrane electrode for Hg(II), having better linear range, wide working pH range (2-4.5) with fast response in the real environment.

  14. High-performance cation-exchange chromatofocusing of proteins.

    PubMed

    Kang, Xuezhen; Frey, Douglas D

    2003-03-28

    Chromatofocusing using high-performance cation-exchange column packings, as opposed to the more commonly used anion-exchange column packings, is investigated with regard to the performance achieved and the range of applications possible. Linear or convex gradients in the range from pH 2.6 to 9 were formed using a variety of commercially available column packings that provide a buffering capacity in different pH ranges, and either polyampholytes or simple mixtures having a small number (three or fewer) of buffering species as the elution buffer. The resolutions achieved using cation-exchange or anion-exchange chromatofocusing were in general comparable, although for certain pairs of proteins better resolution could be achieved using one type of packing as compared to the other, evidently due to the way electrostatic charges are distributed on the protein surface. Several chromatofocusing methods were investigated that take advantage of the acid-base properties of commercially available cation-exchange column packings. These include the use of gradients with a composite shape, the use of very low pH ranges, and the use of elution buffers containing a single buffering species. The advantages of chromatofocusing over ion-exchange chromatography using a salt gradient at constant pH were illustrated by employing the former method and a cation-exchange column packing to separate beta-lactoglobulins A and B, which is a separation reported to be impossible using the latter method and a cation-exchange column packing. Trends in the apparent isoelectric points determined using cation- and anion-exchange chromatofocusing were interpreted using applicable theories. Results of this study indicate that cation-exchange chromatofocusing is a useful technique which is complementary to anion-exchange chromatofocusing and isoelectric focusing for separating proteins at both the analytical and preparative scales.

  15. 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)

  16. 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.

  17. 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

  18. 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.

  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. Cation exchange chromatographic elution and separation of rubidium

    SciTech Connect

    Mehta, V.P.; Khopkar, S.M.

    1982-01-01

    The systematic cation exchange chromatographic separation of rubidium on Dowex 50W-X8 was carried out with mineral acids and their salts as eluants.A selectivity scale for various eluants in terms of the elution constant was devised. Rubidium was separated from a large number of elements in binary mixtures by the process of gradient or selective elutions or selective sorption. The noteworthy feature of the method is the sequential separation of rubidium from alkali as well as alkaline earth elements.

  1. Cirrus Dopant Nano-Composite Coatings

    DTIC Science & Technology

    2014-11-01

    Nickel Phosphorus versus cirrus Zr nano-composite Nickel Phosphorus on Magnesium cirrus wear resistance 590 1025 1,045 0 200 400 600 800...micron duplex Nickel versus cirrus Ti nano- composite Nickel on Mild Steel cirrus corrosion resistance Duplex Ni Cirrus Ti doped Ni 340 430 503 0...100 200 300 400 500 600 HARDNESS (HV) MICROHARDNESS - ELECTROPLATED NICKEL STANDARD DC PLATED DOPED DC PLATED DOPED PULSE PLATED ↑48% 10

  2. 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

  3. Alloyed copper chalcogenide nanoplatelets via partial cation exchange reactions.

    PubMed

    Lesnyak, Vladimir; George, Chandramohan; Genovese, Alessandro; Prato, Mirko; Casu, Alberto; Ayyappan, S; Scarpellini, Alice; Manna, Liberato

    2014-08-26

    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.

  4. 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.

  5. 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.

  6. Inverse optimization of hydraulic, solute transport, and cation exchange parameters using HP1 and UCODE to simulate cation exchange.

    PubMed

    Jacques, Diederik; Smith, Chris; Šimůnek, Jiří; Smiles, David

    2012-11-01

    Reactive transport modeling is a powerful tool to evaluate systems with complex geochemical relations. However, parameters are not always directly measurable. This study represents one of the first attempts to obtain hydrologic, transport and geochemical parameters from an experimental dataset involving transient unsaturated water flow and solute transport, using an automatic inverse optimization (or calibration) algorithm. The data come from previously published, controlled laboratory experiments on the transport of major cations (Na, K, Mg, Ca) during water absorption into horizontal soil columns that were terminated at different times. Experimental data consisted of the depth profiles of water contents (θ), Cl concentrations, and total aqueous and sorbed concentrations of major cations. The dataset was used to optimize several parameters using the reactive transport model, HP1 and the generic optimization code, UCODE. Although the soil hydraulic and solute transport parameters were also optimized, the study focused mainly on the geochemical parameters because the soil columns were constructed from disturbed soil. The cation exchange capacity and the cation exchange coefficients for two exchange models (Gapon and Rothmund-Kornfeld) were optimized. The results suggest that both calibrated models satisfactorily described the experimental data, although the Rothmund-Kornfeld model fit was slightly better. However, information content and surface response analyses indicated that parameters of the Gapon model are well identifiable, whereas those of the Rothmund-Kornfeld model were strongly correlated. The calibrated geochemical parameters were validated using an independent dataset. In agreement with the identifiability analysis, the Gapon approach was better than the Rothmund-Kornfeld model at calculating the observed concentrations of major cations in the soil solution and on the exchange sites.

  7. Quantifying the properties of nano-composites.

    NASA Astrophysics Data System (ADS)

    Daw, Murray; Zhang, Bo; He, Jian; Tritt, Terry

    2008-03-01

    With the proliferation of nano-composites produced for possible thermoelectric application, we ask the question: To what extent is a given nano-composite like other composites? Or, in other words, when do we know that we have something new? To address this we apply the classical theory of composites to specific nano-composites grown and characterized at Clemson. The theory is very simple and assumes explicitly very simple properties of the materials, the most important being Fourier's Law/Ohm's Law. Given this assumption, the theory of composites can be applied to the nano-composites based on what is known of the microstructure. This ``classical'' result then forms the basis by which the properties can be compared to determine if non-classical effects are being observed. One simple theory is the application of rigorous bounds, such as the Hashin-Strikman Bounds which are based only on very simple microstructural descriptors. Another simple theory is the application of FEM, which can be constructed directly from SEM images of the samples using the NIST code ``OOF''. The FEM produces specific predictions for the composite properties. We find that the Hashin-Strikman Bounds are very useful for analyzing the thermal conductivities of composites, but are too loose to be useful for low-temperature electrical conductivity of composites composed of metals and insulators, where the FEM technique can be applied successfully.

  8. Fractionation of strontium isotopes in cation-exchange chromatography

    SciTech Connect

    Oi, Takao; Ogino, Hideki; Kakihana, Hidetake ); Hosoe, Morikazu )

    1992-04-01

    Strontium isotope fractionation has been observed in cation-exchange chromatography of strontium salts. The heavier isotopes have been found enriched at the front parts of displacement-type chromatograms, which means that the heavier isotopes are preferentially fractionated into the solution phase. The average values of the single-stage separation factor (S) minus one per unit mass difference between isotopes have been 1.0 {times} 10{sup {minus}6} for the strontium chloride system, 2.9 {times} 10{sup {minus}6} for the strontium acetate system, and 3.1 {times} 10{sup {minus}6} for the strontium lactate system at 25C. No evidence of the odd-even anomalous isotope effects has been observed. The isotopic reduced partition function ratios (RPFRs) of the strontium species involved in the present study have been estimated; the RPFRs of the complex species have been found to be larger than that of simple hydrated strontium lactate and strontium acetate systems are larger than that of the strontium chloride system.

  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).

  10. 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.

  11. 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.

  12. Alkaline earth metal cation exchange: effect of mobile counterion and dissolved organic matter.

    PubMed

    Indarawis, Katrina; Boyer, Treavor H

    2012-04-17

    The goal of this research was to provide an improved understanding of the interactions between alkaline earth metals and DOM under conditions that are encountered during drinking water treatment with particular focus on cation exchange. Both magnetically enhanced and nonmagnetic cation exchange resins were converted to Na, Mg, Ca, Sr, and Ba mobile counterion forms as a novel approach to investigate the exchange behavior between the cations and the interactions between the cations and DOM. The results show that cation exchange is a robust process for removal of Ca(2+) and Mg(2+) considering competition with cations on the resin surface and presence of DOM. DOM was actively involved during the cation exchange process through complexation, adsorption, and coprecipitation reactions. In addition to advancing the understanding of ion exchange processes for water treatment, the results of this work are applicable to membrane pretreatment to minimize fouling, treatment of membrane concentrate, and precipitative softening.

  13. Ammonia vapor sensing properties of polyaniline-titanium(IV)phosphate cation exchange nanocomposite.

    PubMed

    Khan, Asif Ali; Baig, Umair; Khalid, Mohd

    2011-02-28

    In this study, the electrically conducting polyaniline-titanium(IV)phosphate (PANI-TiP) cation exchange nanocomposite was synthesized by sol-gel method. The cation exchange nanocomposite based sensor for detection of ammonia vapors was developed at room temperature. It was revealed that the sensor showed good reversible response towards ammonia vapors ranging from 3 to 6%. It was found that the sensor with p-toluene sulphonic acid (p-TSA) doped exhibited higher sensing response than hydrochloric acid doped. This sensor has detection limit ≤1% ammonia. The response of resistivity changes of the cation exchange nanocomposite on exposure to different concentrations of ammonia vapors shows its utility as a sensing material. These studies suggest that the cation exchange nanocomposite could be a good material for ammonia sensor at room temperature.

  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

    Sytnyk, Mykhailo; Kirchschlager, Raimund; Bodnarchuk, Maryna I; Primetzhofer, Daniel; Kriegner, Dominik; Enser, Herbert; Stangl, Julian; Bauer, Peter; Voith, Michael; Hassel, Achim Walter; Krumeich, Frank; Ludwig, Frank; Meingast, Arno; Kothleitner, Gerald; Kovalenko, Maksym V; Heiss, Wolfgang

    2013-02-13

    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 Fe(2+) to Co(2+) 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 Co(2+) is demonstrated. By applying the cation exchange to FeO/CoFe(2)O(4) 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.

  16. 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

  17. Preparation of weak cation exchange packings for chromatographic separation of proteins using "click chemistry''.

    PubMed

    Zhao, Kailou; Bai, Quan; Song, Chao; Wang, Fei; Yang, Fan

    2012-04-01

    "Click chemistry" is defined as a class of robust and selective chemical reactions affording high yields and is tolerant to a variety of solvents (including water), functional groups, and air. In this study, click chemistry was used as an effective strategy for coupling three alkyne-carboxylic acids onto the azide-silica to obtain three novel stationary phases of weak cation exchange chromatography, which were characterized with FTIR and elemental analysis. Six kinds of standard proteins, such as myoglobin, RNase A, RNase B, cytochrome C, α-chymotrypsin A, and lysozyme, were separated completely with the three novel weak cation exchange chromatography stationary phases. Compared with commercial weak cation exchange chromatography columns, the three kinds of novel weak cation exchange chromatography packings prepared by click chemistry approach have better resolution and selectivity. The mass recovery of more than 97% was obtained for all the tested proteins, and the bioactivity recovery of lysozyme on the prepared column was determined to be 96%. In addition, lysozyme was purified successfully from egg white with the novel weak cation exchange chromatography column by one step. The purity was more than 97% and a high specific activity was achieved to be 81 435 U/mg. The results illustrate the potential of click chemistry for preparing stationary phase for ion-exchange chromatography.

  18. Polypyrrole, Formation and Use

    DTIC Science & Technology

    2005-01-01

    transformer en un matériau robuste. Parmi les matériaux présentant un tel intérêt, on retrouve des peintures au polypyrrole, des composites moulés... peintures au polypyrrole, des composites moulés par injection de type polypyrrole/poly(chlorure de vinyle) et des tissus et des fibres enduits de polypyrrole

  19. Effect of cation exchange on major cation chemistry in the large scale redox experiment at Aespoe

    SciTech Connect

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

    1994-10-01

    Predicting the chemical changes that result from excavating a repository below the groundwater table in granitic terrain is a major focus of the SKB geochemistry program. The modeling study presented here demonstrates that cation exchange can play a major role in controlling the fluid chemistry that results when groundwaters of differing composition mix due to flow induced by excavation of the HRL tunnel. The major goal of this study was to assess whether an equilibrium cation exchange model could explain the composition of groundwater sampled from boreholes in the HRL tunnel. Given the consistency of the cation exchange hypothesis with observations, geochemical modeling was used to assess whether the quantity of exchanger necessary to match model results and observation was physically reasonable. The impact of mineral dissolution and precipitation on fluid chemistry was also evaluated. Finally, the compositions of exchanger phases expected to be in equilibrium with various Aespoe groundwaters were predicted.

  20. 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.

  1. Computer simulation of displacement cation exchange chromatography: separation of trivalent actinides and lanthanides

    SciTech Connect

    Forsberg, C.W.

    1980-05-01

    A first-generation mathematical model of displacement cation exchange chromatography (CES) was constructed. The model incorporated the following phenomena: diffusion of cations up and down the column, diffusion of cations from the bulk liquid to the resin surface, and equilibrium of cations between liquid and solid resin beads. A limited number of experiments with rare earths using DTPA as the separation agent were undertaken to increase the current understanding of the processes involved in cation exchange chromatography. The numerical computer program based on the mathematical model was written in FORTRAN IV for use on the IBM 360 series of computers.

  2. Kinetic Analysis of Cation Exchange in Birnessite using Time-resolved Synchrotron X-ray Diffraction

    SciTech Connect

    C Lopano; P Heaney; J Bandstra; J Post; S Brantley

    2011-12-31

    In this study, we applied time-resolved synchrotron X-ray diffraction (TRXRD) to develop kinetic models that test a proposed two-stage reaction pathway for cation exchange in birnessite. These represent the first rate equations calculated for cation exchange in layered manganates. Our previous work has shown that the substitution of K, Cs, and Ba for interlayer Na in synthetic triclinic birnessite induces measurable changes in unit-cell parameters. New kinetic modeling of this crystallographic data supports our previously postulated two-stage reaction pathway for cation exchange, and we can correlate the kinetic steps with changes in crystal structure. In addition, the initial rates of cation exchange, R ({angstrom}{sup 3} min{sup -1}), were determined from changes in unit-cell volume to follow these rate laws: R = 1.75[K{sup +}{sub (aq)}]{sup 0.56}, R = 41.1[Cs{sup +}{sub (aq)}]{sup 1.10}, R = 1.15[Ba{sup 2+}{sub (aq)}]{sup 0.50}. Thus, the exchange rates for Na in triclinic birnessite decreased in the order: Cs >> K > Ba. These results are likely a function of hydration energy differences of the cations and the preference of the solution phase for the more readily hydrated cation.

  3. Behavior of human serum albumin on strong cation exchange resins: I. experimental analysis.

    PubMed

    Voitl, Agnes; Butté, Alessandro; Morbidelli, Massimo

    2010-08-20

    Experiments with human serum albumin on the strong cation exchange resin Fractogel EMD SE Hicap (M) were carried out. Even though human serum albumin was used at high purity, two peaks in gradient elution experiments occurred. The obtained data can be explained by considering that human serum albumin binds to Fractogel EMD SE Hicap (M) in two different binding conformations: the protein adsorbs instantaneously in the first conformation and then changes into the second one with a kinetic limitation. The two-peak behavior of human serum albumin was analyzed in detail, especially at various gradient lengths, concentrations and temperatures. Breakthrough curves were performed at four modifier concentrations and three velocities. The characteristic adsorption behavior, found for gradient experiments, was confirmed by the breakthrough curves. The two-peak elution pattern of human serum albumin was also found for other strong cation exchange resins, but not for weak cation exchange resins. It is concluded that the described behavior is peculiar for the interaction of human serum albumin with the strong cation exchange ligand of the resin.

  4. Nongeminate Radiative Recombination of Free Charges in Cation-Exchanged PbS Quantum Dot Films

    SciTech Connect

    Marshall, Ashley R.; Beard, Matthew C.; Johnson, Justin C.

    2016-06-01

    Using photoluminescence (PL) spectroscopy we explore the radiative recombination pathways in PbS quantum dots (QDs) synthesized by two methods. We compare conventionally synthesized PbS from a PbO precursor to PbS synthesized using cation-exchange from CdS QDs. We show that strongly coupled films of PbS QDs from the cation-exchange luminesce with significant efficiency at room temperature. This is in stark contrast to conventional PbS QDs, which have exceedingly weak room temperature emission. Moreover, the power dependence of the emission is quadratic, indicating bimolecular radiative recombination that is reasonably competitive with trap-assisted recombination, a feature previously unreported in coupled PbS QD films. We interpret these results in terms of a greatly reduced defect concentration for cation-exchanged QDs that mitigates the influence of trap-assisted recombination. Cation-exchanged QDs have recently been employed in highly efficient and air-stable lead chalcogenide QD devices, and the reduced number of trap states inferred here may lead to improved current collection and higher open circuit voltage.

  5. A method for the production of weakly acidic cation exchange resins

    NASA Astrophysics Data System (ADS)

    Heller, H.; Werner, F.; Mitschker, A.; Diehl, H. V.; Schaefer, A.

    1991-12-01

    The invention relates to a nonpolluting method for the production of weakly acidic cation exchange resins by saponification of cross-linked acrylonitrile bead polymers, with an alkaline saponification agent at elevated temperature, according to which method the bead polymer and alkaline saponification agent are jointly added only at elevated temperature.

  6. 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...

  7. Manufacture of cellulose nanocrystals by cation exchange resin-catalyzed hydrolysis of cellulose.

    PubMed

    Tang, Li-rong; Huang, Biao; Ou, Wen; Chen, Xue-rong; Chen, Yan-dan

    2011-12-01

    Cellulose nanocrystals (CNC) were prepared from microcrystalline cellulose (MCC) by hydrolysis with cation exchange resin (NKC-9) or 64% sulfuric acid. The cation exchange resin hydrolysis parameters were optimized by using the Box-Behnken design and response surface methodology. An optimum yield (50.04%) was achieved at a ratio of resin to MCC (w/w) of 10, a temperature of 48 °C and a reaction time of 189 min. Electron microscopy (EM) showed that the diameter of CNCs was about 10-40 nm, and the length was 100-400 nm. Regular short rod-like CNCs were obtained by sulfuric acid hydrolysis, while long and thin crystals of cellulose were obtained with the cation exchange resin. X-ray diffraction (XRD) showed that, compared with MCC, the crystallinity of H2SO4-CNC and resin-CNC increased from 72.25% to 77.29% and 84.26%, respectively. The research shows that cation exchange resin-catalyzed hydrolysis of cellulose could be an excellent method for manufacturing of CNC in an environmental-friendly way.

  8. 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.

  9. Fabrication of patterned calcium cross-linked alginate hydrogel films and coatings through reductive cation exchange.

    PubMed

    Bruchet, Marion; Melman, Artem

    2015-10-20

    Calcium cross-linked alginate hydrogels are widely used in targeted drug delivery, tissue engineering, wound treatment, and other biomedical applications. We developed a method for preparing homogeneous alginate hydrogels cross-linked with Ca(2+) cations using reductive cation exchange in homogeneous iron(III) cross-linked alginate hydrogels. Treatment of iron(III) cross-linked alginate hydrogels with calcium salts and sodium ascorbate results in reduction of iron(III) cations to iron(II) that are instantaneously replaced with Ca(2+) cations, producing homogeneous ionically cross-linking hydrogels. Alternatively, the cation exchange can be performed by photochemical reduction in the presence of calcium chloride using a sacrificial photoreductant. This approach allows fabrication of patterned calcium alginate hydrogels through photochemical patterning of iron(III) cross-linked alginate hydrogel followed by the photochemical reductive exchange of iron cations to calcium.

  10. Multicolour synthesis in lanthanide-doped nanocrystals through cation exchange in water

    PubMed Central

    Han, Sanyang; Qin, Xian; An, Zhongfu; Zhu, Yihan; Liang, Liangliang; Han, Yu; Huang, Wei; Liu, Xiaogang

    2016-01-01

    Meeting the high demand for lanthanide-doped luminescent nanocrystals across a broad range of fields hinges upon the development of a robust synthetic protocol that provides rapid, just-in-time nanocrystal preparation. However, to date, almost all lanthanide-doped luminescent nanomaterials have relied on direct synthesis requiring stringent controls over crystal nucleation and growth at elevated temperatures. Here we demonstrate the use of a cation exchange strategy for expeditiously accessing large classes of such nanocrystals. By combining the process of cation exchange with energy migration, the luminescence properties of the nanocrystals can be easily tuned while preserving the size, morphology and crystal phase of the initial nanocrystal template. This post-synthesis strategy enables us to achieve upconversion luminescence in Ce3+ and Mn2+-activated hexagonal-phased nanocrystals, opening a gateway towards applications ranging from chemical sensing to anti-counterfeiting. PMID:27698348

  11. Nutrient leaching from conifer needles in relation to foliar apoplast cation-exchange capacity

    SciTech Connect

    Turner, D.P.; van Broekhuizen, H.J.

    1992-01-01

    Limited evidence to date suggests that acidic precipitation promotes leaching of nutrient cations from conifer foliage. In order to evaluate the relative contribution of the apoplast cation exchange complex and symplast nutrient pools to the leached ions, the magnitude of potential foliar leaching in response to acidic precipitation was compared to foliar apoplast cation exchange capacity (CEC) for two conifer tree species (Pseudotsuga menziesii and Picea engelmanii). Leaching increased with decreasing pH and increasing time of immersion. At pH 2.1 and 3.1, equivalents of H+ depleted from the acidic solutions approximated equivalent of cations gained by the solutions. Maximum amounts leached were less than 40 micro equiv/g dry weight of needles for all ions combined. Measured foliar apoplast CEC for these species was approximately 120 micro equiv/g dry weight of needles. These relative magnitudes indicated that the apoplast provided the leached ions.

  12. Multicolour synthesis in lanthanide-doped nanocrystals through cation exchange in water

    NASA Astrophysics Data System (ADS)

    Han, Sanyang; Qin, Xian; An, Zhongfu; Zhu, Yihan; Liang, Liangliang; Han, Yu; Huang, Wei; Liu, Xiaogang

    2016-10-01

    Meeting the high demand for lanthanide-doped luminescent nanocrystals across a broad range of fields hinges upon the development of a robust synthetic protocol that provides rapid, just-in-time nanocrystal preparation. However, to date, almost all lanthanide-doped luminescent nanomaterials have relied on direct synthesis requiring stringent controls over crystal nucleation and growth at elevated temperatures. Here we demonstrate the use of a cation exchange strategy for expeditiously accessing large classes of such nanocrystals. By combining the process of cation exchange with energy migration, the luminescence properties of the nanocrystals can be easily tuned while preserving the size, morphology and crystal phase of the initial nanocrystal template. This post-synthesis strategy enables us to achieve upconversion luminescence in Ce3+ and Mn2+-activated hexagonal-phased nanocrystals, opening a gateway towards applications ranging from chemical sensing to anti-counterfeiting.

  13. Reactive transport modeling of multicomponent cation exchange at the laboratory and field scale

    SciTech Connect

    Steefel, Carl I.

    2004-04-01

    Multicomponent ion exchange models have been successful in describing the chromatographic separation of cations in both laboratory and field settings. Their chief advantage lies in their ability to capture the competitive effects of other cations that may be present. By incorporating exchanger activity coefficients calculated on the basis of the Gibbs-Duhem equation applied to the exchanger phase, it is possible to correct for the non-ideality of exchange. The use of multiple exchange sites can also substantially improve the ability of the cation exchange models to describe adsorption and retardation. All of these benefits are associated with relatively little additional computational burden. Even where the cost of the multicomponent cation exchange calculations are considered too high, the models are useful in calculating distribution coefficients for the environmental conditions of interest.

  14. Tuning the LSPR in copper chalcogenide nanoparticles by cation intercalation, cation exchange and metal growth.

    PubMed

    Wolf, Andreas; Kodanek, Torben; Dorfs, Dirk

    2015-12-14

    Localized surface plasmon resonances (LSPRs) of degenerately doped copper chalcogenide nanoparticles (NPs) (Cu2-xSe berzelianite and Cu1.1S covellite) have been modified applying different methods. The comparison of the cation exchange (Cu2-xSe) and intercalation (Cu1.1S) of Ag(I) and Cu(I) has shown that Ag(I) causes a non reversible, air stable shift of the LSPR. This was compared to the influence of Au(I) cation exchange into Cu1.1S platelets under the formation of Cu1.1S-Au2S mixed nanoplatelets. Furthermore, we show the growth of Au domains on Cu2-xSe, and discuss the interaction of the two plasmonic parts of the obtained dual plasmonic Cu2-xSe-Au hybrid particles.

  15. [Separation and purification of lysozyme from egg white by high performance cation-exchange chromatography].

    PubMed

    Li, Rong; Chen, Guo-liang

    2002-05-01

    A new method used to separate and purify lysozyme from egg white by high performance cation-exchange chromatography has been established. The process conditions for purifying lysozyme were also discussed in detail. The procedure involved that homogenization of the egg white sample, preliminary purification with sodium chloride, and chromatographic separation by the weak cation exchange column (XIDACE-WCX). The experimental results showed that the purified lysozyme and other impurity proteins were completely separated. By using bioactivity assay, the recovery of lysozyme was 107%, and the specific activity was 15,467 U/mg through the column. Its purity was raised 5.6-fold. The collected fraction with activity was detected by size-exclusion chromatography (SEC). The purified lysozyme was homogeneous. Compared with the traditional soft-based low pressure ion-exchange chromatography, the developed method is rapid and effective.

  16. Novel tetrazole-functionalized ion exchanger for weak cation-exchange chromatography of proteins.

    PubMed

    Lei, Genhu; Xiong, Xiaohu; Wei, Yinmao; Zheng, Xiaohui; Zheng, Jianbin

    2008-04-11

    A new type of weak cation exchanger, tetrazole-functionalized silica, was developed for bioseparation. It was prepared conveniently by modifying silica gel initially with gamma-glycidoxypropyltrimethoxysilane, then with 3-hydroxypropionitrile and finally with ammonium-catalyzed (3+2) azide-nitrile cycloaddition, which is an element of click chemistry. The prepared stationary phase was characterized and evaluated for its separation performance, protein retention behavior, loading capacity, protein recovery and chemical stability. The results show that the stationary phase developed has excellent performance for protein separations with high mass recoveries, and has long-term stability. Some remarkable differences were observed between this new exchanger and a carboxylic methyl-functionalized ion exchanger, which is typically used in weak cation-exchange chromatography of proteins. The obtained column was also used for the purification of lysozyme from chicken egg white, and the purity and specific bioactivity of the obtained lysozyme were about 90% and 67 IU/mg, respectively.

  17. Downstream processing of human antibodies integrating an extraction capture step and cation exchange chromatography.

    PubMed

    Azevedo, Ana M; Rosa, Paula A J; Ferreira, I Filipa; de Vries, J; Visser, T J; Aires-Barros, M Raquel

    2009-01-01

    In this paper we explore an alternative process for the purification of human antibodies from a Chinese hamster ovary (CHO) cell supernatant comprising a ligand-enhanced extraction capture step and cation exchange chromatography (CEX). The extraction of human antibodies was performed in an aqueous two-phase system (ATPS) composed of dextran and polyethylene glycol (PEG), in which the terminal hydroxyl groups of the PEG molecule were modified with an amino acid mimetic ligand in order to enhance the partition of the antibodies to the PEG-rich phase. This capture step was optimized using a design of experiments and a central composite design allowed the determination of the conditions that favor the partition of the antibodies to the phase containing the PEG diglutaric acid (PEG-GA) polymer, in terms of system composition. Accordingly, higher recovery yields were obtained for higher concentrations of PEG-GA and lower concentrations of dextran. The highest yield experimentally obtained was observed for an ATPS composed of 5.17% (w/w) dextran and 8% (w/w) PEG-GA. Higher purities were however predicted for higher concentrations of both polymers. A compromise between yield and purity was achieved using 5% dextran and 10% PEG-GA, which allowed the recovery of 82% of the antibodies with a protein purity of 96% and a total purity of 63%, determined by size-exclusion chromatography. ATPS top phases were further purified by cation exchange chromatography and it was observed that the most adequate cation exchange ligand was carboxymethyl, as the sulfopropyl ligand induced the formation of multi-aggregates or denatured forms. This column allowed the elution of 89% of the antibodies present in the top phase, with a protein purity of 100% and a total purity of 91%. The overall process containing a ligand-enhanced extraction step and a cation exchange chromatography step had an overall yield of 73%.

  18. U/sub 3/O/sub 8/ powder from uranyl-loaded cation exchange resin

    SciTech Connect

    Mosley, W.C.

    1985-01-01

    U/sub 3/O/sub 8/ powder has been produced from uranyl-loaded cation exchange resin with density, particle size distribution, and grain size suitable for powder metallurgy fabrication of reactor fuel tubes with Al-U/sub 3/O/sub 8/ cores. Macroporous sulfonate resin in granular form is used in the process. Resin conversion techniques that were evaluated include batch, rotary, and fluidized bed calcination. 2 refs., 16 figs.

  19. 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.

  20. Type-II nanorod heterostructure formation through one-step cation exchange.

    PubMed

    Chen, Meng-Yu; Hsu, Yung-Jung

    2013-01-07

    A novel one-step cation exchange approach has been developed to prepare ZnO-decorated ZnSe nanorods (ZnSe-ZnO NRs), a prototype type-II semiconductor nanoheterostructure. Because of the staggered band offset which promoted effective charge separation, the as-synthesized ZnSe-ZnO NRs exhibited remarkable photocatalytic activities under visible light illumination, demonstrating their promising potentials in relevant photoconversion applications.

  1. Synthesis of Ultrathin and Thickness-Controlled Cu2-xSe Nanosheets via Cation Exchange.

    PubMed

    Wang, Yuanxing; Zhukovskyi, Maksym; Tongying, Pornthip; Tian, Yang; Kuno, Masaru

    2014-11-06

    We demonstrate the use of cation exchange to synthesize ultrathin and thickness-controlled Cu2-xSe nanosheets (NSs) beginning with CdSe NSs. In this manner, extremely thin (i.e., 1.6 nm thickness) Cu2-xSe NSs, beyond which can be made directly, have been obtained. Furthermore, they represent the thinnest NSs produced via cation exchange. Notably, the exchange reaction preserves the starting morphology of the CdSe sheets and also retains their cubic crystal structure. The resulting nonstoichiometric and cubic Cu2-xSe NSs are stable and do not exhibit any signs of Cu or Se oxidation after exposure to air for 2 weeks. Resulting NSs also show the existence of a localized surface plasmon resonance in the infrared due to the presence of copper vacancies. Efforts to isolate intermediates during the cation exchange reaction show that it occurs via a mechanism where entire sheets are rapidly converted into the final product once the exchange reaction commences, precluding the isolation of alloyed species.

  2. Strong cation-exchange chromatography of proteins on a sulfoalkylated monolithic cryogel.

    PubMed

    Perçin, Işık; Khalaf, Rushd; Brand, Bastian; Morbidelli, Massimo; Gezici, Orhan

    2015-03-20

    A new strong cation exchanger (SCX) monolithic column was synthesized by at-line surface modification of a cryogel prepared by copolymerization of 2-hydroxyethylmethacrylate (HEMA) and glycidylmethacrylate (GMA). Sodium salt of 3-Mercaptopropane sulfonic acid (3-MPS) was used as the ligand to transform the surface of the monolith into a strong cation exchanger. The obtained material was characterized in terms of elemental analysis, infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Brunauer-Emmett-Teller (BET) N2 adsorption, and used as a stationary phase for strong-cation exchange chromatography of some proteins, such as α-chymotrypsinogen, cytochrome c and lysozyme. Water permeability of the column was calculated according to Darcy's law (2.66×10(-13)m(2)). The performance of the monolithic cryogel column was evaluated on the basis of Height Equivalent to a Theoretical Plate (HETP). Retention behavior of the studied proteins was modeled on the basis of Yamamoto model to understand the role of the ion-exchange mechanism in retention behaviors. The considered proteins were successfully separated, and the obtained chromatogram was compared with that obtained with a non-functionalized cryogel column.

  3. 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

  4. Cation exchange in a temporally fluctuating thin freshwater lens on top of saline groundwater

    NASA Astrophysics Data System (ADS)

    Eeman, S.; De Louw, P. G. B.; Van der Zee, S. E. A. T. M.

    2016-10-01

    In coastal-zone fields with a high groundwater level and sufficient rainfall, freshwater lenses are formed on top of saline or brackish groundwater. The fresh and the saline water meet at shallow depth, where a transition zone is found. This study investigates the mixing zone that is characterized by this salinity change, as well as by cation exchange processes, and which is forced by seepage and by rainfall which varies as a function of time. The processes are first investigated for a one-dimensional (1D) stream tube perpendicular to the interface concerning salt and major cation composition changes. The complex sequence of changes is explained with basic cation exchange theory. It is also possible to show that the sequence of changes is maintained when a two-dimensional field is considered where the upward saline seepage flows to drains. This illustrates that for cation exchange, the horizontal component (dominant for flow of water) has a small impact on the chemical changes in the vertical direction. The flow's horizontal orientation, parallel to the interface, leads to changes in concentration that are insignificant compared with those that are found perpendicular to the interface, and are accounted for in the 1D flow tube. Near the drains, differences with the 1D considerations are visible, especially in the longer term, exceeding 100 years. The simulations are compared with field data from the Netherlands which reveal similar patterns.

  5. 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

  6. Tensile/Shear Behaviour of Multi-stitched/Nano Composites

    NASA Astrophysics Data System (ADS)

    Bilisik, Kadir; Kaya, Gaye

    2017-02-01

    This study aims to investigate tensile/shear behavior of multi-stitched/nano composites. For this purpose, non-stitched, non-stitched/nano, multi-stitched and multi-stitched/nano composites were made. It was shown that the warp/filling tensile strength and modulus of composites were slightly reduced in both multi-stitched and multi-stitched/nano composites due to fiber breakage that resulted from the multi-stitching process. In addition, there were not significant differences between non-stitched and multi-stitched structures. The non-stitched/nano composite showed slightly higher in-plane shear strength compared with the non-stitched composite. The in-plane shear strength of the non-stitched composite, on the other hand, increased steadily compared to the multi-stitched composite because of the stitching process and the interface between the stitching yarn and polymer matrix. Stitching significantly improved the delamination resistance in the multi-stitched and multi-stitched/nano composites experienced a small amount of damaged areas. The incorporation of nano silica improved the damage resistance of multi-stitched composites. Therefore, the damaged tolerance composite was developed with stitching and the addition of the nano silica for various industrial applications, such as electronic boards.

  7. 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%.

  8. 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.

  9. 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.

  10. U/sub 3/O/sub 8/ powder from uranyl-loaded cation exchange resin

    SciTech Connect

    Mosley, W.C.

    1985-01-01

    Large batches of U/sub 3/O/sub 8/, suitable for powder metallurgy fabrication of Al-U/sub 3/O/sub 8/ cores for reactor fuel tubes, have been produced by deep-bed calcination of granular uranyl-loaded macroporous sulfonate cation exchange resin at 900 to 950/sup 0/C in air. Deep-bed calcination is the backup process for the reference process of rotary calcination and sintering. These processes are to be used for recycling uranium, and to produce U/sub 3/O/sub 8/ in the Fuel Production Facility to be built at the Savannah River Plant. 2 refs., 6 figs.

  11. A novel configuration of microbial fuel cell stack bridged internally through an extra cation exchange membrane.

    PubMed

    Liu, Zhidan; Liu, Jing; Zhang, Songping; Su, Zhiguo

    2008-06-01

    This paper reports a novel configuration of stacked microbial fuel cells (MFCs) bridged internally through an extra cation exchange membrane (CEM). The MFC stack (MFC(stack)), assembled from two single MFCs (MFC(single)), resulted in double voltage output and half optimal external resistance. COD removal rate was increased from 32.4% to 54.5%. The performance improvement could be attributed to the smaller internal resistance and enhanced cations transfer. A result from a half cell study further confirmed the important role of the extra CEM. This study also demonstrated MFCs where the anode and cathode were sandwiched between two CEMs possessed significantly high power outputs.

  12. Use of cation-exchange resin for the detection of alkylpyridines in beer.

    PubMed

    Peppard, T L; Halsey, S A

    1980-12-19

    A method has been devised whereby trace amounts of certain basic compounds, such as pyridines, may be detected and semi-quantified in beer in the presence of an excess of other flavour constituents including pyrazines. The method involves steam distillation of beer under reduced pressure and subsequent passage of the distillate through a column of weakly acidic Zerolit cation-exchange resin. The resin is eluted with aqueous sodium chloride, the eluate extracted with organic solvent and the concentrated extract analysed by gas chromatography coupled with mass spectrometry. Using this technique with multiple ion detection, a series of alkylpyridines was readily detectable in beers and worts at levels below 1 ppb.

  13. Comparison of cation exchange resins for recovering americium and plutonium from chloride wastes

    SciTech Connect

    Silva, R.A.; Smith, C.M.; Navratil, J.D.; Thompson, G.H.

    1984-04-25

    Macroreticular and microreticular cation exchange resins were compared for their capability of recovering americium and plutonium from solutions of calcium, magnesium, potassium, and sodium chlorides. Americium and plutonium breakthrough capacity and elution behavior of the resins were determined. Of the resins tested, Dowex MSC-1 was selected as the most efficient because of its favorable capacity and excellent elution behavior. Actinide eluting agents were also studied. More concentrated (9.0M) nitric acid was found to elute plutonium faster than 7.0M HNO/sub 3/ used previously, while 7.0M HNO/sub 3/-0.1M NANO/sub 2/ eluted americium fastest.

  14. Strong cation exchange chromatography in analysis of posttranslational modifications: innovations and perspectives.

    PubMed

    Edelmann, Mariola J

    2011-01-01

    Strong cation exchange (SCX) chromatography has been utilized as an excellent separation technique that can be combined with reversed-phase (RP) chromatography, which is frequently used in peptide mass spectrometry. Although SCX is valuable as the second component of such two-dimensional separation methods, its application goes far beyond efficient fractionation of complex peptide mixtures. Here I describe how SCX facilitates mapping of the protein posttranslational modifications (PTMs), specifically phosphorylation and N-terminal acetylation. The SCX chromatography has been mainly used for enrichment of these two PTMs, but it might also be beneficial for high-throughput analysis of other modifications that alter the net charge of a peptide.

  15. Nano-composites for water remediation: a review.

    PubMed

    Tesh, Sarah J; Scott, Thomas B

    2014-09-17

    As global populations continue to increase, the pressure on water supplies will inevitably intensify. Consequently the international need for more efficient and cost effective water remediation technologies will also rise. The introduction of nano-technology into the industry may represent a significant advancement and zero-valent iron nano-particles (INPs) have been thoroughly studied for potential remediation applications. However, the application of water dispersed INP suspensions is limited and somewhat contentious on the grounds of safety, whilst INP reaction mechanisms, transport properties and ecotoxicity are areas still under investigation. Theoretically, the development of nano-composites containing INPs to overcome these issues provides the logical next step for developing nano-materials that are better suited to wide application across the water industry. This review provides an overview of the range of static, bulk nano-composites containing INPs being developed, whilst highlighting the limitations of individual solutions, overall classes of technology, and lack of comparative testing for nano-composites. The review discusses what further developments are needed to optimize nano-composite water remediation systems to subsequently achieve commercial maturity.

  16. 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.

  17. Cation exchange surface-mediated denaturation of an aglycosylated immunoglobulin (IgG1).

    PubMed

    Gillespie, Ron; Nguyen, Thao; Macneil, Sean; Jones, Laurie; Crampton, Shon; Vunnum, Suresh

    2012-08-17

    Cation exchange chromatography of an aglycosylated IgG1 resulted in two distinct peaks during gradient elution. The early eluting peak contained <1% high molecular weight (HMW) species, while the later peak contained 23% HMW species. Analysis by hydrogen-deuterium exchange and Fourier transform infrared spectroscopy (FTIR) indicated that aggregate formation and generation of the second peak were caused by antibody denaturation on the resin surface. Denaturation and HMW generation was increased by the use of strong cation exchange media, by increasing antibody residence time on the exchanger, or increasing temperature. Denaturation and HMW generation was reduced by increasing pH or ionic strength, by the use of preferentially excluded solutes such as citrate or glycine and controlled entirely by addition of 125 mM arginine to the process buffers. This leads to the hypothesis that denaturation and HMW generation of this antibody can be managed by reducing the strength of binding, by increasing its conformational stability, or by suppressing non-native protein-protein interactions. The glycosylated version of this antibody exhibited less than 2% denatured form, suggesting that glycosylation contributes significantly to the stability of this antibody. These findings may be helpful in managing aggregation in other antibodies, and particularly useful in developing purification processes for aglycosylated antibodies.

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

    PubMed

    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.

  19. 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.

  20. The Effects of Elevated CO2 on Soil Respiration, Cation Exchange, and Mineral Dissolution (Invited)

    NASA Astrophysics Data System (ADS)

    Oh, N.; Richter, D. D.

    2010-12-01

    A key weathering agent of the Earth’s crust is soil CO2, produced mainly by plant roots and soil heterotrophs, a water-soluble gas that forms carbonic acid which reacts with soil minerals via cation exchange and mineral dissolution reactions. The elevated atmospheric CO2 can enhance both cation exchange and mineral dissolution reactions through increased plant production and subsequent increase in soil CO2 concentrations. Using laboratory column leaching experiments and field observations of soil water chemistry at the Duke FACE (Free Air CO2 Enrichment) experiment located in a warm temperate climate in North Carolina, USA, we examined the link among elevated atmospheric CO2, soil CO2 concentration, and weathering products in soil water. Results demonstrate that carbonic acid can readily displace exchangeable base cations in soils, altering soil-water chemistry and nutrient availability and also indicating that soil acidification can be enhanced under high CO2 world. The rate and extent at which soil acidification is being promoted by rising CO2 are important research issues for biogeochemistry.

  1. 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.

  2. 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.

  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. Chabazite: stable cation-exchanger in hyper alkaline concrete pore water.

    PubMed

    Van Tendeloo, Leen; Wangermez, Wauter; Kurttepeli, Mert; de Blochouse, Benny; Bals, Sara; Van Tendeloo, Gustaaf; Martens, Johan A; Maes, André; Kirschhock, Christine E A; Breynaert, Eric

    2015-02-17

    To avoid impact on the environment, facilities for permanent disposal of hazardous waste adopt multibarrier design schemes. As the primary barrier very often consists of cement-based materials, two distinct aspects are essential for the selection of suitable complementary barriers: (1) selective sorption of the contaminants in the repository and (2) long-term chemical stability in hyperalkaline concrete-derived media. A multidisciplinary approach combining experimental strategies from environmental chemistry and materials science is therefore essential to provide a reliable assessment of potential candidate materials. Chabazite is typically synthesized in 1 M KOH solutions but also crystallizes in simulated young cement pore water, a pH 13 aqueous solution mainly containing K(+) and Na(+) cations. Its formation and stability in this medium was evaluated as a function of temperature (60 and 85 °C) over a timeframe of more than 2 years and was also asessed from a mechanistic point of view. Chabazite demonstrates excellent cation-exchange properties in simulated young cement pore water. Comparison of its Cs(+) cation exchange properties at pH 8 and pH 13 unexpectedly demonstrated an increase of the KD with increasing pH. The combined results identify chabazite as a valid candidate for inclusion in engineered barriers for concrete-based waste disposal.

  5. 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.

  6. Cation exchange on the nanoscale: an emerging technique for new material synthesis, device fabrication, and chemical sensing.

    PubMed

    Rivest, Jessy B; Jain, Prashant K

    2013-01-07

    Cation exchange is an age-old technique for the chemical conversion of liquids or extended solids by place-exchanging the cations in an ionic material with a different set of cations. The technique is undergoing a major revival with the advent of high-quality nanocrystals: researchers are now able to overcome the limitations in bulk systems and fully exploit cation exchange for materials synthesis and discovery via rapid, low-temperature transformations in the solid state. In this tutorial review, we discuss cation exchange as a promising materials synthesis and discovery tool. Exchange on the nanoscale exhibits some unique attributes: rapid kinetics at room temperature (orders of magnitude faster than in the bulk) and the tuning of reactivity via control of nanocrystal size, shape, and surface faceting. These features make cation exchange a convenient tool for accessing nanocrystal compositions and morphologies for which conventional synthesis may not be established. A simple exchange reaction allows extension of nanochemistry to a larger part of the periodic table, beyond the typical gamut of II-VI, IV-VI, and III-V materials. Cation exchange transformations in nanocrystals can be topotactic and size- and shape-conserving, allowing nanocrystals synthesized by conventional methods to be used as templates for production of compositionally novel, multicomponent, or doped nanocrystals. Since phases and compositions resulting from an exchange reaction can be kinetically controlled, rather than governed by the phase diagram, nanocrystals of metastable and hitherto inaccessible compositions are attainable. Outside of materials synthesis, applications for cation exchange exist in water purification, chemical staining, and sensing. Since nanoscale cation exchange occurs rapidly at room temperature, it can be integrated with sensitive environments such as those in biological systems. Cation exchange is already allowing access to a variety of new materials and processes

  7. 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

  8. 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.

  9. 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.

  10. Comparison of chromatographic ion-exchange resins V. Strong and weak cation-exchange resins.

    PubMed

    Staby, Arne; Jacobsen, Jan H; Hansen, Ronni G; Bruus, Ulla K; Jensen, Inge Holm

    2006-06-23

    Strong and weak cation-exchangers were compared for a number of chromatographic parameters, i.e. pH dependence, efficiency, binding strength, particle size distribution, static and dynamic capacity, and scanning electron microscopy (SEM) pictures. Chromatographic resins investigated were Fractogel EMD SO3- (M), Fractogel EMD SE Hicap (M), Fractogel EMD COO- (M), MacroPrep 25S, MacroPrep High S, MacroPrep CM, CM HyperZ, and Matrex Cellufine C-500. Testing was done with three proteins: Anti-FVII Mab (IgG), aprotinin, and lysozyme. For lysozyme and aprotinin with pI above experimental pH, dependence of pH on retention was generally low, though some pronounced decrease of retention with increasing pH was observed for CM HyperZ. For Anti-FVII Mab with pI<7.5, binding was observed on several resins at pH 7.5. Efficiency results present the expected trend of increasing dependence of plate height as a function of increasing flow rate, and the highest flow dependence was observed for Fractogel EMD COO-. Particle size distribution was determined by two independent methods, coulter counting and SEM pictures, with fair agreement. Binding strength data of cation-exchange resins as a function of ionic strength depends on the protein, but binding and elution at high salt concentration may in general be performed with MacroPrep resins. Comparison of dynamic capacity data at 10% break-through and static capacity measurements shows that a very diverse utilization of approximately 25-90% of the total available capacity is employed during chromatographic operation. The effect of competitive binding from yeast fermentation components on dynamic binding capacity of aprotinin was studied showing a significant decrease in binding capacity. Sepharose FF, Toyopearl 650 M, and Ceramic HyperD F strong and weak cation-exchange resins were included in this study. Resins with good pure aprotinin capacity also performed well for aprotinin in fermentation broth, but the highest relative capacity

  11. 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.

  12. 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

  13. Behavior of human serum albumin on strong cation exchange resins: II. model analysis.

    PubMed

    Voitl, Agnes; Butté, Alessandro; Morbidelli, Massimo

    2010-08-20

    Experiments with human serum albumin on a strong cation exchange resin exhibit a peculiar elution pattern: the protein elutes with two peaks in a modifier gradient. This behavior is modeled with a general rate model, where the two elution peaks are modeled with two binding conformations, one of which is at equilibrium conditions, while for the other, the adsorption process is rate limited. Isocratic experiments under nonadsorbing conditions were used to characterize the mass transfer process. The isotherm of both adsorption conformations as well as the kinetic of adsorption and desorption for the second conformation are functions of the modifier concentration. They are evaluated with linear modifier gradient experiments and step experiments with various adsorption times. All experimental features are well reproduced by the proposed modified general rate model.

  14. 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

  15. 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.

  16. SLC24A5, a putative cation exchanger, affects pigmentation in zebrafish and humans.

    PubMed

    Lamason, Rebecca L; Mohideen, Manzoor-Ali P K; Mest, Jason R; Wong, Andrew C; Norton, Heather L; Aros, Michele C; Jurynec, Michael J; Mao, Xianyun; Humphreville, Vanessa R; Humbert, Jasper E; Sinha, Soniya; Moore, Jessica L; Jagadeeswaran, Pudur; Zhao, Wei; Ning, Gang; Makalowska, Izabela; McKeigue, Paul M; O'donnell, David; Kittles, Rick; Parra, Esteban J; Mangini, Nancy J; Grunwald, David J; Shriver, Mark D; Canfield, Victor A; Cheng, Keith C

    2005-12-16

    Lighter variations of pigmentation in humans are associated with diminished number, size, and density of melanosomes, the pigmented organelles of melanocytes. Here we show that zebrafish golden mutants share these melanosomal changes and that golden encodes a putative cation exchanger slc24a5 (nckx5) that localizes to an intracellular membrane, likely the melanosome or its precursor. The human ortholog is highly similar in sequence and functional in zebrafish. The evolutionarily conserved ancestral allele of a human coding polymorphism predominates in African and East Asian populations. In contrast, the variant allele is nearly fixed in European populations, is associated with a substantial reduction in regional heterozygosity, and correlates with lighter skin pigmentation in admixed populations, suggesting a key role for the SLC24A5 gene in human pigmentation.

  17. Cobalt determination in natural waters using cation-exchange liquid chromatography with luminol chemiluminescence detection

    SciTech Connect

    Boyle, E.A.; Handy, B.; van Geen, A.

    1987-06-01

    A method has been developed for the analysis of cobalt in natural waters by cation-exchange liquid chromatography using chemiluminescence detection. Cobalt can be determined directly in freshwater samples on 500-..mu..L samples with a detection limit of 20 pmol/kg; larger samples provide proportionately lower detection limits. Seawater samples can be analyzed on 100-mL samples following APDC solvent extraction; the detection limit of this method is 5 pmol/kg. The precision of the method is +/- 5%. The method should also be applicable to the analysis of V, Cu, and Fe in natural waters. Equipment is low in cost and transportable and can be used in the field.

  18. 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.

  19. 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.

  20. Analysis of chromite by cation-exchange using ethylenediaminetetra-acetic acid.

    PubMed

    Jawaid, M; Ingman, F

    1975-12-01

    A method for the separation and determination of five major elements in chromite ore (and chrome-bearing refractories), based on complexation of the metals with EDTA is described. After removal of silica, the cations are separated into two groups by passing the solution through a cation-exchange resin (Dowex 50W-X8, in Na-form) in the presence of an excess of the complexing agent. The optimum conditions for the separation are discussed on the basis of exchange constants that were either known or determined. The first group contains Cr and Fe, which emerge in the filtrate at pH between 1.5 and 2.1, whereas A1, Mg and Ca, which are adsorbed on the resin, form another group. Complexometric titrations are used for the subsequent determination of the cations in each group. The method is simpler and more rapid and accurate for routine analysis than the current methods.

  1. 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.

  2. Comparison of cation exchange resins for recovering americium and plutonium from chloride salts

    SciTech Connect

    Silva, R.A.; Navratil, J.D.

    1983-01-01

    Macroreticular and microreticular cation exchange resins were compared for their capability of recovering americium and plutonium from solutions of calcium, magnesium, potassium, and sodium chlorides. Americium and plutonium breakthrough capacity and elution behavior of the resins were determined. Of the resins tested, Dowex MSC-1 was selected as the most efficient because of its favorable capacity and excellent elution behavior. Actinide eluting agents were also studied. More concentrated (9.0M) nitric acid was found to elute plutonium faster than 7.0M HNO/sub 3/ used previously while 7.0M HNO/sub 3/-0.1M NaNO/sub 2/ eluted americium fastest. 4 tables.

  3. Release of quantum dot nanoparticles in porous media: role of cation exchange and aging time.

    PubMed

    Torkzaban, Saeed; Bradford, Scott A; Wan, Jiamin; Tokunaga, Tetsu; Masoudih, Arash

    2013-10-15

    Understanding the fate and transport of engineered nanoparticles (ENPs) in subsurface environments is required for developing the best strategy for waste management and disposal of these materials. In this study, the deposition and release of quantum dot (QD) nanoparticles were studied in saturated sand columns. The QDs were first deposited in columns using 100 mM NaCl or 2 mM CaC12 solutions. Deposited QDs were then contacted with deionized (DI) water and/or varying Na(+) concentrations to induce release. QDs deposited in 100 mM Na(+) were easily reversible when the column was rinsed with DI water. Conversely, QDs deposited in the presence of Ca(2+) exhibited resistance to release with DI water. However, significant release occurred when the columns were flushed with NaCl solutions. This release behavior was explained by cation exchange (Ca(2+) in exchange sites were replaced by Na(+)) which resulted in the breakdown of calcium bridging. We also studied the effect of aging time on the QD release. As the aging time increased, smaller amounts of QDs were released following cation exchange. However, deposited QDs were subsequently released when the column was flushed with DI water. The release behavior was modeled using a single first-order kinetic release process and changes in the maximum solid phase concentration of deposited QDs with transition in solution chemistry. The results of this study demonstrate that the presence of carboxyl groups on ENPs and divalent ions in the solution plays a key role in controlling ENP mobility in the subsurface environment.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. In situ electrochemical solid-phase extraction of anions and cations using polypyrrole and overoxidized sulfonated polypyrrole.

    PubMed

    Sahin, Yücel; Ercan, Betül; Sahin, Mutlu

    2008-04-15

    A new method for the extraction of both anions and cations is proposed using electro-synthesized polypyrrole (PPy) and overoxidized sulfonated polypyrrole film (OSPPy). In situ anion (chloride, nitrate, sulfate) and cation (calcium, magnesium) uptake and release were examined under controlled potential conditions for prospective applications in electrochemically controlled solid-phase extraction (EC-SPE). The PPy film was used as an anode (anion-exchanger) and OSPPy film was used as a cathode (cation-exchanger) material and reverse order of the electrodes were investigated in EC-SPE. This new cell arrangement containing two ion exchanger polymer electrodes was developed to provide in situ removal of both anions and cations from aqueous solution. Simple preparation of the film coatings on a platinum plate was possible using a constant potential method. Applied positive and negative potentials facilitated the in situ extraction and desorption of ions, respectively. Both anions and cations were desorbed into sample aliquot and were determined by ion chromatography (IC). The method was validated using a standard reference material and tested for the determination of the ions in real water samples.

  9. 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.

  10. 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.

  11. 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.

  12. Positioning of Platinum Nanoparticles In Cation-exchange Membrane By Galvanic Reaction

    NASA Astrophysics Data System (ADS)

    Kumar, Rakesh; Pandey, A. K.; Ramagiri, S. V.; Bellare, J. R.; Goswami, A.

    2010-12-01

    Platinum nanoparticles were formed at the surface of the poly (perfluorosulfonic) acid membrane (Nafion-117) by the galvanic reaction of PtCl62- ions with Ag nanoparticles positioned near the surface of the membrane. The reduction with BH4- ions produced Ag nanoparticles (15±4 nm size) mostly positioned near the surface of membrane due to Donnan exclusion of co-ions (BH4-). Energy Dispersive X-ray Fluorescence (EDXRF) analysis of the membrane indicated that galvanic reaction proceeded quantitatively. Transmission Electron Microscopy (TEM) of the cross-sections of membrane samples indicated that the spherical Pt nanoparticles having size 2 to 8 nm were mostly located near the surface of the membrane. The positioning of Pt nanoparticles at surface of the membrane is important for using nano-composite in catalytical application.

  13. 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

  14. Similar cation exchange capacities among bryophyte species refute a presumed mechanism of peatland acidification.

    PubMed

    Soudzilovskaia, N A; Cornelissen, J H C; During, H J; van Logtestijn, R S P; Lang, S I; Aerts, R

    2010-09-01

    Fen-bog succession is accompanied by strong increases of carbon accumulation rates. We tested the prevailing hypothesis that living Sphagna have extraordinarily high cation exchange capacity (CEC) and therefore acidify their environment by exchanging tissue-bound protons for basic cations in soil water. As Sphagnum invasion in a peatland usually coincides with succession from a brown moss-dominated alkaline fen to an acidic bog, the CEC of Sphagna is widely believed to play an important role in this acidification process. However, Sphagnum CEC has never been compared explicitly to that of a wide range of other bryophyte taxa. Whether high CEC directly leads to the ability to acidify the environment in situ also remains to be tested. We screened 20 predominant subarctic bryophyte species, including fen brown mosses and bog Sphagna for CEC, in situ soil water acidification capacity (AC), and peat acid neutralizing capacity (ANC). All these bryophyte species possessed substantial CEC, which was remarkably similar for brown mosses and Sphagna. This refutes the commonly accepted idea of living Sphagnum CEC being responsible for peatland acidification, as Sphagnum's ecological predecessors, brown mosses, can do the same job. Sphagnum AC was several times higher than that of other bryophytes, suggesting that CE (cation exchange) sites of Sphagna in situ are not saturated with basic cations, probably due to the virtual absence of these cations in the bog water. Together, these results suggest that Sphagna can not realize their CEC in bogs, while fen mosses can do so in fens. The fen peat ANC was 65% higher than bog ANC, indicating that acidity released by brown mosses in the CE process was neutralized, maintaining an alkaline environment. We propose two successional pathways indicating boundaries for a fen-bog shift with respect to bryophyte CEC. In neither of them is Sphagnum CE an important factor. We conclude that living Sphagnum CEC does not play any considerable role

  15. Comparison of chromatographic ion-exchange resins. III. Strong cation-exchange resins.

    PubMed

    Staby, Arne; Sand, Maj-Britt; Hansen, Ronni G; Jacobsen, Jan H; Andersen, Line A; Gerstenberg, Michael; Bruus, Ulla K; Jensen, Inge Holm

    2004-04-23

    A comparative study was performed on strong cation-exchangers to investigate the pH dependence, efficiency, binding strength, particle size distribution, static and dynamic capacity, and SEM pictures of chromatographic resins. The resins tested included: SP Sepharose XL, Poros 50 HS, Toyopearl SP 550c, SP Sepharose BB, Source 30S, TSKGel SP-5PW-HR20, and Toyopearl SP 650c. Testing was performed with four different proteins: anti-FVII Mab (IgG), aprotinin, lysozyme, and myoglobin. Dependence of pH on retention was generally very low for proteins with high pI. An unexpected binding at pH 7.5 of anti-FVII Mab with pI < 7.5 was observed on several resins. Efficiency results show the expected trend of higher dependence of the plate height with increasing flow rate of soft resins compared to resins for medium and high-pressure operation. Determination of particle size distribution by two independent methods, Coulter counting and SEM, was in very good agreement. The mono-dispersed nature of Source 30S was confirmed. Binding to cation-exchange resins as a function of ionic strength varies depending on the specific protein. Generally, binding and elution at high salt concentration may be performed with Toyopearl SP 550c and Poros 50 HS, while binding and elution at low salt concentration may be performed with Toyopearl SP 650c. A very high binding capacity was obtained with SP Sepharose XL. Comparison of static capacity and dynamic capacity at 10% break-through shows in general approximately 50-80% utilisation of the total available capacity during chromatographic operation. A general good agreement was obtained between this study and data obtained by others. The results of this study may be used for selection of resins for testing in process development. The validity of experiments and results with model proteins were tested using human insulin precursor in pure state and in real feed-stock on Toyopearl SP 550c, SP Sepharose BB, and Toyopearl SP 650c. Results showed good

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

    PubMed

    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.

  17. Adsorptional removal of methylene blue by guar gum-cerium (IV) tungstate hybrid cationic exchanger.

    PubMed

    Gupta, V K; Pathania, Deepak; Singh, Pardeep; Kumar, Amit; Rathore, B S

    2014-01-30

    Guar gum-cerium (IV) tungstate nanocomposite (GG/CTNC) cationic exchanger was synthesized using simple sol gel method. The GG/CTNC was characterized using X-ray diffraction (XRD), Fourier transmission infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and energy dispersive X-ray spectrophotometer (EDX). The XRD studies confirmed amorphous and fibrous in nature of GG/CTNC. The high percentage of oxygen in the nanocomposite material confirmed the functionality tungstate (WO4(-)). The ion exchange capacity of GG/CTNC for Na(+) ion was observed to be 1.30 mequivg(-1). The hybrid exchanger was used as potential adsorbent for the removal of methylene blue (MB) from aqueous system. The correlation coefficients value indicated a good fit of monolayer Langmuir model to the adsorption of methylene blue onto GG/CTNC. The adsorption kinetic study revealed that the adsorption process followed the pseudo second order kinetic. The Gibbs free energy (ΔG) values confirmed the spontaneous nature of adsorption process.

  18. Synthesis of high capacity cation exchangers from a low-grade Chinese natural zeolite.

    PubMed

    Wang, Yifei; Lin, Feng

    2009-07-30

    The Chinese natural zeolite, in which clinoptilolite coexists with quartz was treated hydrothermally with NaOH solutions, either with or without fusion with NaOH powder as pretreatment. Zeolite Na-P, Na-Y and analcime were identified as the reacted products, depending on the reaction conditions such as NaOH concentration, reaction time and hydrothermal temperature. The products were identified by X-ray diffraction, and characterized by Fourier transform IR and ICP. With hydrothermal treatment after fusion of natural zeolite with NaOH, high purity of zeolite Na-Y and Na-P can be selectively formed, their cation exchange capacity (CEC) are 275 and 355 meq/100g respectively, which are greatly higher than that of the natural zeolite (97 meq/100g). Furthermore, the ammonium removal by the synthetic zeolite Na-P in aqueous solution was also studied. The equilibrium isotherms have been got and the influence of other cations present in water upon the ammonia uptake suggested an order of preference Ca(2+)>K(+)>Mg(2+).

  19. On-line cation-exchange preconcentration and capillary electrophoresis coupled by tee joint interface.

    PubMed

    Zhang, Zhao-Xiang; He, You-Zhao

    2005-02-25

    An on-line preconcentration method based on ion exchange solid phase extraction was developed for the determination of cationic analytes in capillary electrophoresis (CE). The preconcentration-separation system consisted of a preconcentration capillary bonded with carboxyl cation-exchange stationary phase, a separation capillary for zone electrophoresis and a tee joint interface of the capillaries. Two capillaries were connected closely inside a 0.3 mm i.d. polytetrafluoroethylene tube with a side opening and fixed together by the interface. The preparations of the preconcentration capillaries and interface were described in detail in this paper. The on-line preconcentration and separation procedure of the analysis system included washing and conditioning the capillaries, loading analytes, filling with buffer solution, eluting analytes and separating by capillary zone electrophoresis (CZE). Several analysis parameters, including sample loading flow rate and time, eluting solution and volume, inner diameter and length of preconcentration capillary etc., were investigated. The proposed method enhanced the detection sensitivity of CE-UV about 5000 times for propranolol and metoprolol compared with normally electrokinetic injection. The detection limits of propranolol and metoprolol were 0.02 and 0.1 microg/L with the proposed method respectively, whereas those were 0.1 and 0.5 mg/L with conventional electrokinetic injection. The experiment results demonstrate that the proposed technique can increase the preconcentration factor evidently.

  20. 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.

  1. 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.

  2. 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.

  3. Design of a strong cation exchange methodology for the evaluation of charge heterogeneity in glatiramer acetate.

    PubMed

    Campos-García, Víctor R; López-Morales, Carlos A; Benites-Zaragoza, Eleuterio; Jiménez-Miranda, Armando; Espinosa-de la Garza, Carlos E; Herrera-Fernández, Daniel; Padilla-Calderón, Jesús; Pérez, Néstor O; Flores-Ortiz, Luis F; Medina-Rivero, E

    2017-01-05

    Complex pharmaceuticals are in demand of competent analytical methods able to analyze charge heterogeneity as a critical quality attribute (CQA), in compliance with current regulatory expectations. A notorious example is glatiramer acetate (GA), a complex polypeptide mixture useful for the treatment of relapsing-remitting multiple sclerosis. This pharmaceutical challenges the current state of analytical technology in terms of the capacity to study their constituent species. Thus, a strong cation exchange methodology was designed under the lifecycle approach to support the establishment of GA identity, trough the evaluation of its chromatographic profile, which acts as a charge heterogeneity fingerprint. In this regard, a maximum relative margin of error of 5% for relative retention time and symmetry factor were proposed for the analytical target profile. The methodology met the proposed requirements after precision and specificity tests results, the former comprised of sensitivity and selectivity. Subsequently, method validation was conducted and showed that the method is able to differentiate between intact GA and heterogeneity profiles coming from stressed, fractioned or process-modified samples. In summary, these results provide evidence that the method is adequate to assess charge heterogeneity as a CQA of this complex pharmaceutical.

  4. 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.

  5. Vacancy ion-exclusion chromatography of haloacetic acids on a weakly acidic cation-exchange resin.

    PubMed

    Helaleh, Murad I H; Tanaka, Kazuhiko; Mori, Masanobu; Xu, Qun; Taoda, Hiroshi; Ding, Ming-Yu; Hu, Wenzhi; Hasebe, Kiyoshi; Haddad, Paul R

    2003-05-16

    A new and simple approach is described for the determination of the haloacetic acids (such as mono-, di- and trichloroacetic acids) usually found in drinking water as chlorination by-products after disinfection processes and acetic acid. The new approach, termed vacancy ion-exclusion chromatography, is based on an ion-exclusion mechanism but using the sample solution as the mobile phase, pure water as the injected sample, and a weakly acidic cation-exchange resin column (TSKgel OApak-A) as the stationary phase. The addition of sulfuric acid to the mobile phase results in highly sensitive conductivity detection with sharp and well-shaped peaks, leading to excellent and efficient separations. The elution order was sulfuric acid, dichloroacetic acid, monochloroacetic acid, trichloroacetic acid, and acetic acid. The separation of these acids depends on their pKa values. Acids with lower pKa values were eluted earlier than those with higher pKa, except for trichloroacetic acid due to a hydrophobic-adsorption effect occurring as a side-effect of vacancy ion-exclusion chromatography. The detection limits of these acids in the present study with conductivity detection were 3.4 microM for monochloroacetic acid, 0.86 microM for dichloroacetic acid and 0.15 microM for trichloroacetic acid.

  6. 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

  7. 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.

  8. Simultaneous Isolation of Lactoferrin and Lactoperoxidase from Bovine Colostrum by SPEC 70 SLS Cation Exchange Resin

    PubMed Central

    Liang, Yafei; Wang, Xuewan; Wu, Mianbin; Zhu, Wanping

    2011-01-01

    In this work, simultaneous isolation of lactoferrin (Lf) and lactoperoxidase (Lp) from defatted bovine colostrum by one-step cation exchange chromatography with SPEC 70 SLS ion-exchange resin was investigated. A RP-HPLC method for Lf and Lp determination was developed and optimized as the following conditions: detection wavelength of 220 nm, flow rate of 1 mL/min and acetonitrile concentration from 25% to 75% within 20 min. The adsorption process of Lf on SPEC 70 SLS resin was optimized using Lf standard as substrate. The maximum static binding capacity of SPEC 70 SLS resin was of 22.0 mg/g resin at 15 °C, pH 7.0 and adsorption time 3 h. The Lf adsorption process could be well described by the Langmuir adsorption isotherm model, with a maximum adsorption capacity of 21.73 mg/g resin at 15 °C. In batch fractionation of defatted colostrum, the binding capacities of SPEC 70 SLS resin for adsorbing Lf and Lp simultaneously under the abovementioned conditions were 7.60 and 6.89 mg/g resin, respectively, both of which were superior to those of CM Sepharose F.F. or SP Sepharose F.F. resins under the same conditions. As a result, SPEC 70 SLS resin was considered as a successful candidate for direct and economic purification of Lf and Lp from defatted colostrum. PMID:22016715

  9. [Interactions between proteins and cation exchange adsorbents analyzed by NMR and hydrogen/deuterium exchange technique].

    PubMed

    Wang, Kang; Hao, Dongxia; Qi, Shuting; Ma, Guanghui

    2014-09-01

    In silico acquirement of the accurate residue details of protein on chromatographic media is a bottleneck in protein chromatography separation and purification. Here we developed a novel approach by coupling with H/D exchange and nuclear magnetic resonance to observe hen egg white lysozyme (HEWL) unfolding behavior adsorbed on cation exchange media (SP Sepharose FF). Analysis of 1D 1H-NMR shows that protein unfolding accelerated H/D exchange rate, leading to more loss of signal of amide hydrogen owing to exposure of residues and the more unfolding of protein. Analysis of two-dimensional hydrogen-hydrogen total correlation spectroscopy shows that lysozyme lost more signals and experienced great unfolding during its adsorption on media surface. However, for several distinct fragments, the protection degrees varied, the adsorbed lysozyme lost more signal intensity and was less protected at disorder structures (coil, bend, and turn), but was comparatively more protected against exchange at secondary structure domains (α-helix, β-sheet). Finally, the binding site was determined by electrostatic calculations using computer simulation methods in conjunction with hydrogen deuterium labeled protein and NMR. This study would help deeply understand the microscopic mechanism of protein chromatography and guide the purposely design of chromatographic process and media. Moreover, it also provide an effective tool to study the protein and biomaterials interaction in other applications.

  10. 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.

  11. Semiautomated method for cation-exchange capacity determination of reservoir rocks

    SciTech Connect

    Gall, B.L.; Raible, C.J.; Volk, L.J.

    1983-04-01

    The presence of significant amounts of clay in tight-gas sand formations makes the determination of cation exchange capacities (CEC) important for electric-log, self potential (SP), and gamma ray log interpretation. In the past, CEC measurements have been difficult and time-consuming to obtain. However, an automated method that avoids many difficulties of other techniques while determining the CEC's of many samples at one time has been described by Worthington. This work is a modification of the work done by Worthington. Easily assembled commercial equipment instead of specially built equipment is used to agitate rock samples contained in dialysis membrane bags during ion exchange with barium acetate solution and during washing of the samples to remove excess barium ions. Barium acetate is used as the source of barium ions instead of barium chloride, which is used in Worthington's procedure, to avoid corrosion of the stainless steel equipment. The amount of barium ions on the rock samples is then determined by conductometric titration with magnesium sulfate. The titration procedure is not automated. In addition, the use of the barium ion method was extended to samples with CEC values an order of magnitude lower than those determined by Worthington. Most measured CEC's for the western tight-gas sands ranged from 0.5 to 10 meq/100 g with a few to 19 meg/100 g. A comparison of barium acetate, adsorbed water, and ammonium acetate methods for determining CEC's is made.

  12. Semiautomated method for cation-exchange capacity determination of reservoir rocks

    SciTech Connect

    Gall, B.L.; Raible, C.J.; Volk, L.J.

    1983-04-01

    The presence of significant amounts of clay in tight-gas sand formations makes the determination of cation exchange capacities (CEC) important for electric-log, self potential (SP), and gamma ray log interpretation. In the past, CEC measurements have been difficult and time-consuming to obtain. However, an automated method that avoids many difficulties of other techniques while determining the CEC's of many samples at one time has been described by Worthington. This work is a modification of the work done by Worthington. Easily assembled commercial equipment instead of specially built equipment is used to agitate rock samples contained in dialysis membrane bags during ion exchange with barium acetate solution and during washing of the samples to remove excess barium ions. Barium acetate is used as the source of barium ions instead of barium chloride, which is used in Worthington's procedure, to avoid corrosion of the stainless steel equipment. The amount of barium ions on the rock samples is then determined by conductometric titration with magnesium sulfate. The titration procedure is not automated. In addition, the use of the barium ion method was extended to samples with CEC values an order of magnitude lower than those determined by Worthington.

  13. Nature identification and morphology characterization of cation-exchange membrane fouling during conventional electrodialysis.

    PubMed

    Ayala-Bribiesca, Erik; Pourcelly, Gérald; Bazinet, Laurent

    2006-08-15

    The aim of this work was to study the effect of a concentrate solution pH value and of the composition in calcium, carbonate, and protein of a diluate solution to be treated by conventional electrodialysis on the fouling of cation-exchange membranes (CEM). It appeared that after demineralization of solutions containing CaCl(2) and CaCl(2)+Na(2)CO(3) using a concentrate solution maintained at a pH of 12, mineral fouling appeared on both sides of the CEM. The nature of the deposits was identified as calcium hydroxide and/or carbonate on both surfaces. The mineral fouling presented an aggregation-like crystal following a carnation-like pattern of aggregates of small rhombohedral crystals with CaCl(2) added alone, while CaCl(2)+Na(2)CO(3) yielded a smoother spherical crystal. Protein fouling was detected only on the CEM surface in contact with the diluate after demineralization of a solution containing CaCl(2)+Na(2)CO(3) using a concentrate pH value of 2.

  14. 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.

  15. 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.

  16. Oxidative decomposition properties of cationic exchange resins producing SO4(2-) in power plants.

    PubMed

    Zhu, Zhiping; Dai, Chenlin; Liu, Sen; Tian, Ye

    2015-01-01

    The sulphate content of a system increases when strong-acid cationic exchange resins leak into a system or when sulphonic acid groups on the resin organic chain detach. To solve this problem, a dynamic cycle method was used in dissolution experiments of several resins under H2O2 or residual chlorine conditions. Results show that after performing dynamic cycle experiments for 120 hours under oxidizing environments, the SO4(2-) and total organic carbon (TOC) released by four kinds of resins increased with time, contrary to their release velocity. The quantity of released SO4(2-) increased as the oxidizing ability of oxidants was enhanced. Results showed that the quantity and velocity of released SO4(2-) under residual chlorine condition were larger than those under H2O2 condition. Data analysis of SO4(2-) and TOC released from the four kinds of resins by the dynamic cycle experiment revealed that the strength of oxidation resistance of the four resins were as follows: 650C>1500H>S200>SP112H.

  17. Cation exchange displacement batch chromatography of proteins guided by screening of protein purification parameters.

    PubMed

    Kotasińska, Marta; Richter, Verena; Thiemann, Joachim; Schlüter, Hartmut

    2012-11-01

    Displacement chromatography has been shown to be an effective alternative for protein purification. We investigated in this study sample displacement chromatography, which does not require a displacer molecule. Furthermore, we performed a screening for determination of parameters for an optimal sample displacement chromatography. We screened the affinities of cytochrome C, lysozyme, myoglobin, and ribonuclease A toward a cation exchange material as a function of different pH values and to presence of different concentrations of sodium chloride in the sample application buffer. Sample displacement chromatography in batch chromatography mode for the separation of the protein mixture was studied with a sample application buffer with a pH of 5 and 7. As predicted by the screening experiments, sample displacement chromatography was most effective at pH 7 since this pH guaranteed the largest differences of the affinities of the four proteins toward the stationary phase. In summary, we describe here sample displacement chromatography in the batch chromatography mode for the separation of proteins, which is a simple and fast alternative to conventional displacement chromatography. Systematic screening of chromatographic parameters prior to sample displacement chromatography promises a successful separation of a target protein.

  18. Kinetics of Isovalent (Cd(2+)) and Aliovalent (In(3+)) Cation Exchange in Cd1-xMnxSe Nanocrystals.

    PubMed

    Chakraborty, Pradip; Jin, Yu; Barrows, Charles J; Dunham, Scott T; Gamelin, Daniel R

    2016-10-05

    Ion exchange, in which an in-diffusing ion replaces a lattice ion, has been widely exploited as a synthetic tool for semiconductor doping and solid-to-solid chemical transformations, both in bulk and at the nanoscale. Here, we present a systematic investigation of cation-exchange reactions that involve the displacement of Mn(2+) from CdSe nanocrystals by Cd(2+) or In(3+). For both incoming cations, Mn(2+) displacement is spontaneous but thermally activated, following Arrhenius behavior over a broad experimental temperature range. At any given temperature, cation exchange by In(3+) is approximately 2 orders of magnitude faster than that by Cd(2+), illustrating a critical dependence on the incoming cation. Quantitative analysis of the kinetics data within a Fick's-law diffusion model yields diffusion barriers (ED) and limiting diffusivities (D0) for both incoming ions. Despite their very different kinetics, indistinguishable diffusion barriers of ED ≈ 1.1 eV are found for both reactions (In(3+) and Cd(2+)). A dramatically enhanced diffusivity is found for Mn(2+) cation exchange by In(3+). Overall, these findings provide unique experimental insights into cation diffusion within colloidal semiconductor nanocrystals, contributing to our fundamental understanding of this rich and important area of nanoscience.

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

    PubMed

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

    2012-07-19

    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.

  20. Weak cation-exchange restricted-access material for on-line purification of basic drugs in plasma.

    PubMed

    Sato, Yoshiaki; Yamamoto, Eiichi; Takakuwa, Susumu; Kato, Takashi; Asakawa, Naoki

    2008-05-09

    A methylcellulose-immobilized weak cation-exchange (MC-WCX) silica-based restricted-access material (RAM) was developed. The MC-WCX consists of an MC outer surface and 2-carboxyethyl phase internal surface, allowing for direct analysis of basic drugs in plasma. The retention properties of the MC-WCX were evaluated for sulpiride, quinidine, ranitidine, and desipramine. The MC-WCX retained model drugs by cation-exchange, and retained drugs were eluted with the mobile phase containing small amount of acids or salts compared with the MC strong cation-exchanger (MC-SCX). These results indicated the ease of use of the MC-WCX solid-phase extraction (SPE) column when coupled to a reversed-phase analytical column in column-switching high-performance liquid chromatography (HPLC), and various detection principals. Further direct analysis of model drugs in plasma using the MC-WCX SPE column in a column-switching HPLC system successfully performed with sufficient recovery. It is concluded that the MC-WCX is useful for the analysis of basic drugs in plasma.

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

    PubMed

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

    2011-01-01

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

  2. 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%.

  3. 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.

  4. 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.

  5. Adsorption characteristics and the kinetics of the cation exchange of rhodamine-6G with Na+-montmorillonite.

    PubMed

    Gemeay, Ali H

    2002-07-15

    The adsorption and the kinetics of the cation exchange of rhodamine-6G (Rh-6G) with Na(+)-montmorillonite (Na(+)-MMT) have been studied. The binding parameters of Rh-6G have been determined by applying Freundlich and D-R isotherms. The enthalpy and the entropy of adsorption have been determined. The isosteric heat of adsorption has also been determined and decreases with increasing the concentration of Rh-6G. Increasing the concentration of Rh-6G led to a decrease in the adsorption capacity, which attributed to the formation of Rh-6G aggregates. Kinetic measurements of the cation exchange were followed up using a stopped-flow electrical conductivity detection unit. The cation-exchange process exhibited first-order kinetics with respect to the dye concentration and inversely proportional to the clay concentration. The measurements were accomplished at different temperatures and the activation parameters were determined. Increasing the Na(+)-MMT concentration led to a decrease in the rate constant. The latter is also affected by changing the exchangeable cation.

  6. Cation-exchange behavior of berkelium in aqueous-organic solutions of nitric acid, containing trioctylphosphine oxide

    SciTech Connect

    Guseva, L.I.; Tikhomirova, G.S.; Korovaikov, P.A.

    1995-07-01

    Behavior of transplutonium elements (TPEs), Eu, and Zr on Dowex-50 cation-exchange resin in aqueous-organic solutions of HNO{sub 3} containing trioctylphosphine oxide (TOPO) has been studied as influenced by the nature of the solvent (H{sub 2}O, CH{sub 3}OH, C{sub 2}H{sub 5}OH, CH{sub 3}COOH, CH{sub 3}CN), the composition and concentration of various components of the solution, and the presence of an oxidant (PbO{sub 2}) in the resin phase. The authors found that the factors of Bk distribution between the PbO{sub 2}-containing resin and CH{sub 3}CN-HNO{sub 3}-TOPO solutions are considerably lower than the distribution factors of other TPEs, which is due to oxidation of Bk(III) into Bk(IV). This fact can be used for separation of Bk(IV) from other TPEs with a cation-exchange column containing an oxidant. The optimal conditions of separation (elution with solutions containing 1.0-2.5 M HNO{sub 3}, 0.1 M TOPO, and 80-90% CH{sub 3}CN) have been determined. A mechanism is proposed for TPE sorption on the cation-exchange resin from aqueous-organic solutions of HNO{sub 3} containing TOPO. The analogy between behavior of TPEs in ion-exchange and extraction processes in these systems is discussed.

  7. Adsorption of deamidated antibody variants on macroporous and dextran-grafted cation exchangers: II. Adsorption kinetics.

    PubMed

    Tao, Yinying; Carta, Giorgio; Ferreira, Gisela; Robbins, David

    2011-03-18

    Single and multicomponent batch adsorption kinetics were obtained for deamidated mAb variants on two commercial cation exchangers, one with an open macroporous structure--UNOsphere S--and the other with charged dextran grafts--Capto S. The adsorption kinetics for the macroporous matrix was found to be controlled largely by pore diffusion. The effective diffusivity estimated from single component data was a fraction of the mAb free solution diffusivity, and its value could be used to accurately predict the adsorption kinetics for two- and three-component systems. In this case, when two or more variants were adsorbed simultaneously, both experimental and predicted results showed a temporary overshoot of the amount adsorbed above the equilibrium value for the more deamidated variant followed by a gradual approach to equilibrium. Adsorption rates on the dextran grafted material were much faster than those observed for the macroporous matrix for both single component and simultaneous adsorption cases. In this case, no significant overshoot was observed for the more deamidated forms. The Capto S adsorption kinetics could be described well by a diffusion model with an adsorbed phase driving force for single component adsorption and for the simultaneous adsorption of multiple variants. However, this model failed to predict the adsorption kinetics when more deamidated forms pre-adsorbed on the resin were displaced by less deamidated ones. In this case, the kinetics of the displacement process was much slower indicating that the pre-adsorbed components severely hindered transport of the more strongly bound variants. Overall, the results indicate that despite the lower capacity, the macroporous resin may be more efficient in process applications where displacement of one variant by another takes place as a result of the faster and more predictable kinetics.

  8. Cation Exchange Resins and colonic perforation. What surgeons need to know

    PubMed Central

    Rodríguez-Luna, María Rita; Fernández-Rivera, Enrique; Guarneros-Zárate, Joaquín E.; Tueme-Izaguirre, Jorge; Hernández-Méndez, José Roberto

    2015-01-01

    Introduction Since 1961 the use of Cation Exchange Resins has been the mainstream treatment for chronic hyperkalemia. For the past 25 years different kind of complications derived from its clinical use have been recognized, being the colonic necrosis the most feared and lethal of all. Presentation of case We report a case of a 72-year-old patient with chronic kidney disease, treated with calcium polystyrene sulfonate for hyperkalemia treatment who presented in the emergency department with constipation treated with hypertonic cathartics. With clinical deterioration 48 h later progressed with colonic necrosis requiring urgent laparotomy, sigmoidectomy and open abdomen management with subsequent rectal stump perforation and dead. The histopathology finding: calcium polystyrene sulfonate embedded in the mucosa, consistent with the cause of perforation. Discussion Lillemoe reported the first case series of five uremic patients with colonic perforation associated with the use of SPS in sorbitol in 1987 and in 2009 the FDA removed from the market the SPS containing 70% of sorbitol. The pathophysiologic change of CER goes from mucosal edema, ulcers, pseudomembranes, and the most severe case transmural necrosis. Up to present day, some authors have questioned the use of CER in the setting of lowering serum potassium. Despite its worldwide use in hyperkalemia settings, multiple studies have not demonstrated a significant potassium excretion by CER. Conclusion Despite the low incidence of colonic complication and lethal colonic necrosis associated with the CER clinical use, the general surgeon needs a high index of suspicion when dealing with patients treated with CER and abdominal pain. PMID:26439420

  9. Sorption mechanism and predictive models for removal of cationic organic contaminants by cation exchange resins.

    PubMed

    Jadbabaei, Nastaran; Zhang, Huichun

    2014-12-16

    Understanding the sorption mechanism of organic contaminants on cation exchange resins (CXRs) will enable application of these resins for the removal of cationic organic compounds from contaminated water. In this study, sorption of a diverse set of 12 organic cations and 8 neutral aromatic solutes on two polystyrene CXRs, MN500 and Amberlite 200, was examined. MN500 showed higher sorbed concentrations due to its microporous structure. The sorbed concentrations followed the same trend of aromatic cations > aliphatic cations > neutral solutes for both resins. Generally, solute-solvent interactions, nonpolar moiety of the solutes, and resin matrix can affect selectivity of the cations. Sorbed concentrations of the neutral compounds were significantly less than those of the cations, indicating a combined effect of electrostatic and nonelectrostatic interactions. By conducting multiple linear regression between Gibbs free energy of sorption and Abraham descriptors for all 20 compounds, polarity/polarizability (S), H-bond acidity (A), induced dipole (E), and electrostatic (J(+)) interactions were found to be involved in the sorption of the cations by the resins. After converting the aqueous sorption isotherms to sorption from the ideal gas-phase by water-wet resins, a more significant effect of J(+) was observed. Predictive models were then developed based on the linear regressions and validated by accurately estimating the sorption of different test set compounds with a root-mean-square error range of 0.91-1.1 and 0.76-0.85 for MN500 and Amberlite 200, respectively. The models also accurately predicted sorption behavior of aniline and imidazole between pH 3 and 10.

  10. Sn cation valency dependence in cation exchange reactions involving Cu(2-x)Se nanocrystals.

    PubMed

    De Trizio, Luca; Li, Hongbo; Casu, Alberto; Genovese, Alessandro; Sathya, Ayyappan; Messina, Gabriele C; Manna, Liberato

    2014-11-19

    We studied cation exchange reactions in colloidal Cu(2-x)Se nanocrystals (NCs) involving the replacement of Cu(+) cations with either Sn(2+) or Sn(4+) 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 Cu(2-x)Se NCs remains cubic regardless of the degree of copper deficiency (that is, "x") in the NC lattice. Also, Sn(4+) ions are comparable in size to the Cu(+) ions, while Sn(2+) 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 Sn(4+) cations are used, alloyed Cu(2-4y)Sn(y)Se 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 Sn(4+) cations would require a drastic reorganization of the anion framework, which is not possible at the reaction conditions of the experiments. When instead Sn(2+) 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 Cu(2-x)Se/SnSe heterostructures, with no Cu-Sn-Se alloys.

  11. 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

  12. Alkali recovery using PVA/SiO2 cation exchange membranes with different -COOH contents.

    PubMed

    Hao, Jianwen; Gong, Ming; Wu, Yonghui; Wu, Cuiming; Luo, Jingyi; Xu, Tongwen

    2013-01-15

    By changing -COOH content in poly(acrylic acid-co-methacryloxypropyl trimethoxy silane (poly(AA-co-γ-MPS)), a series of PVA/SiO(2) cation exchange membranes are prepared from sol-gel process of poly(AA-co-γ-MPS) in presence of poly(vinyl alcohol) (PVA). The membranes have the initial decomposition temperature (IDT) values of 236-274 °C. The tensile strength (TS) ranges from 17.4 MPa to 44.4 MPa. The dimensional stability in length (DS-length) is in the range of 10%-25%, and the DS-area is in the range of 21%-56% in 65 °C water. The water content (W(R)) ranges from 61.2% to 81.7%, the ion exchange capacity (IEC) ranges from 1.69 mmol/g to 1.90 mmol/g. Effects of -COOH content on diffusion dialysis (DD) performance also are investigated for their potential applications. The membranes are tested for recovering NaOH from the mixture of NaOH/Na(2)WO(4) at 25 - 45 °C. The dialysis coefficients of NaOH (U(OH)) are in the range of 0.006-0.032 m/h, which are higher than those of the previous membranes (U(OH): 0.0015 m/h, at 25 °C). The selectivity (S) can reach up to 36.2. The DD performances have been correlated with the membrane structure, especially the continuous arrangement of -COOH in poly(AA-co-γ-MPS) chain.

  13. 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.

  14. Sulfate ion (SO4(2-)) release from old and new cation exchange resins used in condensate polishing systems for power plants.

    PubMed

    Zhu, Zhi-Ping; Tang, Xue-Ying; Yin, Zhao-Hui; Yu, Wei-Wei

    2014-01-01

    In this study, a dynamic cycle test, a static immersion method and a pyrolysis experiment were combined to examine the characteristics of SO4(2-) released from several new and old cation exchange resins used in condensate polishing systems for power plants. The results show that the quantity and velocity of SO4(2-) released from new and old resins tend to balance in a short time during the dynamic cycle experiment. SO4(2-) is released by 1500H (monosphere super gel type cation exchange resins) and 001 × 7 (gel type cation exchange resins) new and old cation exchange resins, the quantity of which increases according to immersion time. In the pyrolysis experiment, the quantity of SO4(2-) released from resins increases and the pH of the pyrolysis solution transforms from alkaline to acidic with an increase in temperature.

  15. Novel nano-composite biomaterials that respond to light.

    PubMed

    Hribar, Kolin C; Metter, Robert B; Burdick, Jason A

    2009-01-01

    Composites of nanoparticles and polymers are finding wide applications to alter material properties, conductivity, and utility. Here, we show that nano-composites can be designed to heat in the presence of near infrared light. This process is useful in transitioning materials through a transition temperature for a range of applications. For example, shape-memory materials (including polymers, metals, and ceramics) are those that are processed into a temporary shape and respond to some external stimuli (e.g., temperature) to undergo a transition back to a permanent shape and may be useful in a range of applications from aerospace to fabrics, to biomedical devices and microsystem components. In this work, we formulated composites of gold nanorods (<1% by volume) and biodegradable networks, where exposure to infrared light induced heating and consequently, shape transitions. The heating is repeatable and tunable based on nanorod concentration and light intensity.

  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. NIR determination of Cation Exchange Capacity and Exchangeable Cations of Italian Corn Areas Soils

    NASA Astrophysics Data System (ADS)

    Cabassi, G.; Piombino, M.; Orfeo, D.; Marino Gallina, P.

    2009-04-01

    The determinations of cation exchange capacity (CSC ) and exchangeable cations of soils using conventional wet methods are time consuming and require skilled analysts in order to obtain both precise and accurate results. Aim of this work was to evaluate NIR reflectance spectroscopy in order to obtain a rapid estimate of these soil parameters. A representative and heterogeneous set of 250 soil samples was selected from a population of soils sampled in all the northern Italy corn areas for which the organic carbon content and the texture were known. In order to maximize CSC variability the model of Courtin et al. (1979, CSC=23+3680*Organic Carbon+510*Clay) was used to estimate the CSC of selected samples. The true CSC was determined using the Barium Chloride-Triethanolamine at pH 8.1 method, and the the exchangeable cations were analyzed by atomic absorption spectroscopy. The results are summarized in table 1: MinMax meanStandard deviationAnalytical error CSC (meq(+)/kg)3.5 90.9 20.6 14.3 0.75 Ca (mg/kg) 220 215933366 2689 97.5 Mg (mg/kg) 18 1483 300 240 7.8 K (mg/kg) 61 1058 273 169 7.9 The NIR spectra on dry soil ground at 0.5 mm were acquired using a FOSS 5000 spectrometer. In order to maximize the calibration performances and to select the smallest calibration set were tested two multivariate design of experiment techniques: Kennard-Stone algorithm (KS) and Neighborhood Mahlanobis Distance (NMD). The regression model built with using NMD design and a Neighborhood distance of 0.5 gave a standard error of prediction of 4.6 cmol(+)/kg and a R2 of 0.853 using 139 sample in calibration set and 111 samples in validation set. For exchangeable Ca, Mg and K the standard error of prediction were 738, 98 and 136 mg/kg and the R2 were 0.837, 0.714 and 0.230 respectively. These results demonstrated the usefulness of the NIR technique for rough determination of CSC and divalent exchangeable cations on heterogeneous soils.

  18. Sulphonic acid strong cation-exchange restricted access columns in sample cleanup for profiling of endogenous peptides in multidimensional liquid chromatography. Structure and function of strong cation-exchange restricted access materials.

    PubMed

    Machtejevas, E; Denoyel, R; Meneses, J M; Kudirkaite, V; Grimes, B A; Lubda, D; Unger, K K

    2006-08-04

    In this work, the pore structural parameters and size exclusion properties of LiChrospher strong cation-exchange and reverse phase restricted access materials (RAM) are analysed. The molecular weight size exclusion limit for polystyrenes was found to be about 17.7 kDa, while for standard proteins, the molecular weight size exclusion limit was higher, at approximately 25 kDa. The average pore diameter on a volume basis calculated from the pore network model changes from 8.5 nm (native LiChrospher) to 8.6 nm (diol derivative) to 8.2 nm (sulphonic acid derivative) to 6.9 nm (n-octadecyl derivative). Additional characterisations were performed on restricted access materials with nitrogen sorption at 77 K, water adsorption at 25 degrees C, intrusion-extrusion of water (in order to evaluate the hydrophobic properties of the pores of the hydrophobic RAM), and zeta potential measurements by microelectrophoresis. For peptide analysis out of the biofluids, the strong cation-exchange functionality seems to be particularly suitable mainly because of the high loadability of the strong cation-exchange restricted access material (SCX-RAM) and the fact that one can work under non-denaturing conditions to perform effective chromatographic separations. For bacitracin, the dynamic capacity of the SCX-RAM columns does not reach its maximum value in the analysed range. For lysozyme, the dynamic capacity reaches a value of 0.08 mg/ml of column volume before column is overloaded. Additionally, the proper column operating conditions that lead to the total effective working time of the RAM column to be equal to approximately 500 injections (depending on the type of sample), is comprehensively described. The SCX-RAM column was used in the same system analysing urine samples for the period of 1 month (approximately 150 injections) with run-to-run reproducibility below 5% RSD and below 10% RSD for the relative fractions.

  19. 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

  20. Cu3-x P Nanocrystals as a Material Platform for Near-Infrared Plasmonics and Cation Exchange Reactions.

    PubMed

    De Trizio, Luca; Gaspari, Roberto; Bertoni, Giovanni; Kriegel, Ilka; Moretti, Luca; Scotognella, Francesco; Maserati, Lorenzo; Zhang, Yang; Messina, Gabriele C; Prato, Mirko; Marras, Sergio; Cavalli, Andrea; Manna, Liberato

    2015-02-10

    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-x P 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-x P NCs. It is likely that both the LSPR and the p-type character of our Cu3-x P 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-x P NCs as a starting material on which to probe cation exchange reactions. We demonstrate here that Cu3-x P NCs can be easily cation-exchanged to hexagonal wurtzite InP NCs, with preservation of the anion framework (the anion framework in Cu3-x P is very close to that of wurtzite InP). Intermediate steps in this reaction are represented by Cu3-x P/InP heterostructures, as a consequence of the fact that the exchange between Cu(+) and In(3+) ions starts from the peripheral corners of each NC and gradually evolves toward the center. The feasibility of this transformation makes Cu3-x P NCs an interesting material platform from which to access other metal phosphides by cation exchange.

  1. 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

  2. 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

  3. Modelling of geochemical reactions and experimental cation exchange in MX 80 bentonite.

    PubMed

    Montes-H, G; Fritz, B; Clement, A; Michau, N

    2005-10-01

    Bentonites are widely used for waste repository systems because of their hydrodynamic, surface and chemical-retention properties. MX 80 bentonite (bentonite of Wyoming) contains approximately 85% Na/Ca-montmorillonite and 15% accessory minerals. The dominant presence of Na/Ca-montmorillonite in this clay mineral could cause it to perform exceptionally well as an engineered barrier for a radioactive waste repository because this buffer material is expected to fill up by swelling the void between canisters containing waste and the surrounding ground. However, the Na/Ca-montmorillonite could be transformed to other clay minerals as a function of time under repository conditions. Previous modelling studies based on the hydrolysis reactions have shown that the Na/Ca-montmorillonite-to-Ca-montmorillonite conversion is the most significant chemical transformation. In fact, this chemical process appears to be a simple cation exchange into the engineered barrier. The purpose of the present study was two-fold. Firstly, it was hoped to predict the newly formed products of bentonite-fluid reactions under repository conditions by applying a thermokinetic hydrochemical code (KIRMAT: Kinetic Reactions and Mass Transport). The system modelled herein was considered to consist of a 1-m thick zone of water-saturated engineered barrier. This non-equilibrated system was placed in contact with a geological fluid on one side, which was then allowed to diffuse into the barrier, while the other side was kept in contact with iron-charged water. Reducing initial conditions ( [P(O)2 approximately equals 0] ; Eh=-200 mV) and a constant reaction temperature (100 degrees C) were considered. Secondly, it was hoped to estimate the influence of inter-layer cations (Ca and Na) on the swelling behaviour of the MX 80 bentonite by using an isothermal system of water vapour adsorption and an environmental scanning electron microscope (ESEM) coupled with a digital image analysis (DIA) program. Here, the

  4. On the Structure-Property Relationships of Cation-Exchanged ZK-5 Zeolites for CO2 Adsorption.

    PubMed

    Pham, Trong D; Hudson, Matthew R; Brown, Craig M; Lobo, Raul F

    2017-03-09

    The CO2 adsorption properties of cation-exchanged Li-, Na-, K-, and Mg-ZK-5 zeolites were correlated to the molecular structures determined by Rietveld refinements of synchrotron powder X-ray diffraction patterns. Li-, K-, and Na-ZK-5 all exhibited high isosteric heats of adsorption (Qst ) at low CO2 coverage, with Na-ZK-5 having the highest Qst (ca. 49 kJ mol(-1) ). Mg(2+) was located at the center of the zeolite hexagonal prism with the cation inaccessible to CO2 , leading to a much lower Qst (ca. 30 kJ mol(-1) ) and lower overall uptake capacity. Multiple CO2 adsorption sites were identified at a given CO2 loading amount for all four cation-exchanged ZK-5 adsorbents. Site A at the flat eight-membered ring windows and site B/B* in the γ-cages were the primary adsorption sites in Li- and Na-ZK-5 zeolites. Relatively strong dual-cation adsorption sites contributed significantly to an enhanced electrostatic interaction for CO2 in all ZK-5 samples. This interaction gives rise to a migration of Li(+) and Mg(2+) cations from their original locations at the center of the hexagonal prisms toward the α-cages, in which they interact more strongly with the adsorbed CO2 .

  5. Study of cation-exchange capacity of soil near fluorspar mining with special reference to Kadipani mine (Gujarat, India).

    PubMed

    Pradhan, Alka; Deshmukh, Jitendra P

    2011-10-01

    One of the important functions of soil is exchange of cations, whereby essential trace metals are made available to plants as nutrients. Both minerals and organics fractions of soil exchange the cations. Clay minerals exchange cation because of the presence of negatively charged sites on the mineral while organic materials exchange cations by means of their carboxylate groups and other basic functional groups. Cation exchange in soil provides trace metal nutrients to plant. The metal ions are taken up by the roots while H+ is exchanged for the metal ions. Therefore, the measurement of Cation Exchange Capacity (CEC) of soil is important and this becomes more significant when the mining activity is carried out in the surrounding environment as mining activity may adversely impact the soil texture and organic matter content and sometimes changes the pH which is the main regulator of CEC in soil. The studies related to the assessment of CEC of soil were carried out. 14 soil samples, including one sample of mine site, were collected during summer season from different villages within 10 km radius from the mine site. These samples were then analyzed. The efforts were made to establish the CEC of soil quality of Kadipani, Distt. Vadodara, Gujarat, India. This study is useful for making the decisions regarding the environmental measures required for mining activity.

  6. Sorption of doubly charged metal ions from ammonium fluoride solutions by KFP-23 cation-exchange resin

    SciTech Connect

    Ganyaev, V.P.; Pimneva, L.A.; Pakholkov, V.S.

    1982-10-20

    This report examines the results of a study of sorption of a number of doubly charged cations by the macroporous cation-exchange KFP-12 from 0.1 N MeF/sub 2/ solutions containing NH/sub 4/F in concentrations from 0 to 3.0 M. As the result of an investigation of the sorption, under dynamic conditions, of copper, zinc, cadmium, manganese, cobalt, and nickel ions from ammonium fluoride solutions by KFP-12 cation-exchange resin in the influence of the ionic form (H/sup +/ or NH/sub 4//sup +/) of the resin and of the NH/sub 4/F concentration on the degree of sorption and on the breakthrough capacity was established. The character of bonding and coordination of the sorbed cations with the ionic groups of the resin has been established. The possibilty of thorough purification of ammonium fluoride and (NH/sub 4/)/sub 2/BeF/sub 4/ solutions with the aid of KFP-12 resin in NH/sub 4//sup +/ form has been demonstrated. The purification co-efficients were calculated.

  7. Polymer monoliths with low hydrophobicity for strong cation-exchange capillary liquid chromatography of peptides and proteins.

    PubMed

    Gu, Binghe; Li, Yun; Lee, Milton L

    2007-08-01

    Two polymer monoliths were designed and synthesized from commercially available monomers with an attempt to decrease hydrophobicity for strong cation-exchange chromatography. One was prepared from the copolymerization of sulfoethyl methacrylate and poly(ethylene glycol) diacrylate, and the other was synthesized from vinylsulfonic acid and poly(ethylene glycol) diacrylate. Both of the monoliths were synthesized inside 75-microm i.d., UV-transparent fused-silica capillaries by photopolymerization. The hydrophobicities of the two monoliths were systematically evaluated using standard synthetic undecapeptides under ion-exchange conditions and propyl paraben under reversed-phase conditions. The poly(sulfoethyl methacrylate) monolith demonstrated similar hydrophobicity as a monolith prepared from copolymerization of 2-acrylamido-2-methyl-1-propanesulfonic acid and poly(ethylene glycol) diacrylate, and 40% acetonitrile was required to suppress any hydrophobic interactions with peptides under ion-exchange conditions. However, with the use of vinylsulfonic acid as the functional monomer, a monolith with very low hydrophobicity was obtained, making it suitable for strong cation-exchange liquid chromatography of both peptides and proteins. It was found that monolith hydrophobicity could be adjusted by selection of monomers that differ in hydrocarbon content and type of vinyl group. Finally, excellent separations of model protein standards and high-density lipoproteins were achieved using the poly(vinylsulfonic acid) monolith. Five subclasses of high-density lipoproteins were resolved using a simple linear NaCl gradient.

  8. 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.

  9. [Research on removal of copper, manganese and zinc ions using cation exchange membrane based on Donnan dialysis].

    PubMed

    Xie, De-Hua; Shi, Zhou; Chen, Shi-Yang; Xie, Peng; Song, Yong

    2010-09-01

    Based on Donnan dialysis technique, the mechanism that influences the exchange capacity of the membrane and the interaction mechanism between two co-existing ions are investigated in this paper, where the cation exchange membrane is applied to remove the heavy metal ions such as copper, manganese, zinc. The following results were obtained: It is applicable to use the cation exchange membrane to remove copper, manganese and zinc ions and 75%-85% of removal efficiency can be obtained; when the concentration and charge number are the same, the smaller the radius of hydrated heavy metal, the quicker the ion diffuse and consequently the higher removal efficiency the membrane can achieve, which is the main factor; when the radius of the hydrated heavy metals are approximately same, the membrane will have higher removal efficiency to the ion with lower atomic number; when the ions with same charge number and concentration co-exist, both of them are removed but with different removal speeds for existing of disturbance between them and there exist diffusion competition, i.e. those who are more prone to be exchanged will be more competitive and more likely to low the removal rate of the other ion seriously; if the total concentration of the ions is far lower than the exchange capacity of the membrane, the removal efficiency when the ions coexist is not lower too much than that of the case when they exist lonely.

  10. Indirect UV detection-ion-exclusion/cation-exchange chromatography of common inorganic ions with sulfosalicylic acid eluent.

    PubMed

    Kozaki, Daisuke; Mori, Masanobu; Nakatani, Nobutake; Arai, Kaori; Masuno, Tomoe; Koseki, Masakazu; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2013-01-01

    Herein, we describe indirect UV detection-ion-exclusion/cation-exchange chromatography (IEC/CEC) on a weakly acidic cation-exchange resin in the H(+)-form (TSKgel Super IC-A/C) using sulfosalicylic acid as the eluent. The goal of the study was to characterize the peaks detected by UV detector. The peak directions of analyte ions in UV at 315 nm were negative because the molar absorbance coefficients of analyte anions and cations were lower than that of the sulfosalicylic acid eluent. Good chromatographic resolution and high signal-to-noise ratios of analyte ions were obtained for the separations performed using 1.1 mM sulfosalicylic acid and 1.5 mM 18-crown-6 as the eluent. The relative standard deviations (RSDs) of the peak areas ranged from 0.6 to 4.9%. Lower detection limits of the analytes were achieved using indirect UV detection at 315 nm (0.23 - 0.98 μM) than those obtained with conductometric detection (CD) (0.61 - 2.1 μM) under the optimized elution conditions. The calibration curves were linear in the range from 0.01 to 1.0 mM except for Cl(-), which was from 0.02 to 2.0 mM. The present method was successfully applied to determine common inorganic ions in a pond water sample.

  11. 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.

  12. Comparison of gaseous oxidized Hg measured by KCl-coated denuders, and nylon and cation exchange membranes.

    PubMed

    Huang, Jiaoyan; Miller, Matthieu B; Weiss-Penzias, Peter; Gustin, Mae Sexauer

    2013-07-02

    The chemical compounds that make up gaseous oxidized mercury (GOM) in the atmosphere, and the reactions responsible for their formation, are not well understood. The limitations and uncertainties associated with the current method applied to measure these compounds, the KCl-coated denuder, are not known due to lack of calibration and testing. This study systematically compared the uptake of specific GOM compounds by KCl-coated denuders with that collected using nylon and cation exchange membranes in the laboratory and field. In addition, a new method for identifying different GOM compounds using thermal desorption is presented. Different GOM compounds (HgCl2, HgBr2, and HgO) were found to have different affinities for the denuder surface and the denuder underestimated each of these compounds. Membranes measured 1.3 to 3.7 times higher GOM than denuders in laboratory and field experiments. Cation exchange membranes had the highest collection efficiency. Thermodesorption profiles for the release of GOM compounds from the nylon membrane were different for HgO versus HgBr2 and HgCl2. Application of the new field method for collection and identification of GOM compounds demonstrated these vary as a function of location and time of year. Understanding the chemistry of GOM across space and time has important implications for those developing policy regarding this environmental contaminant.

  13. Separation of macro-quantities of actinide elements at Savannah River by high-pressure cation exchange

    SciTech Connect

    Burney, G.A.

    1980-05-01

    Large-scale separation of actinides from fission products and from each other by pressurized cation exchange chromatography at Savannah River is reviewed. Several kilograms of /sup 244/Cm have been separated, with each run containing as much as 150 g of /sup 244/Cm. Dowex 50W-X8 (Dow Chemical Co.) cation resin, graded to 30-70 micron size range, is used, and separation is made by eluting with 0.05M diethylenetriamine pentaacetic acid (DTPA) at a pH of 3. The effluent from the column is continuously monitored by a BF/sub 3/ detector, a NaI detector, and a lithium-drifted germanium detector and gamma spectrometer to guide collection of product fractions. Operating the columns at 300 to 1000 psi pressure eliminates resin bed disruption caused by radiolytically produced gases, and operating at increased flow rates decreases the radiolytic degradation of the resin per unit of product processed. A portion of the hot canyon of a production radiochemical separation plant was converted from a remote crane-operated facility to a master-slave manipulator-operated facility for separation and purification of actinide elements by pressurized cation exchange. It also contains an evaporator, furnaces, a calorimeter, and several precipitators and associated tanks. Actinide processing from target dissolution to packaging of purified product is planned in this facility.

  14. 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.

  15. 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.

  16. Lysozyme-Mediated Formation of Protein-Silica Nano-Composites for Biosensing Applications (Postprint)

    DTIC Science & Technology

    2009-05-05

    reagents Lysozyme (from hen egg white ), tetramethyl orthosilicate (TMOS) and tetraethyl orthosilicate (TEOS) were purchased from Sigma–Aldrich (St. Louis...AFRL-RX-TY-TP-2009-4611 LYSOZYME -MEDIATED FORMATION OF PROTEIN-SILICA NANO-COMPOSITES FOR BIOSENSING APPLICATIONS (POSTPRINT) Madhumati...Include area code) 15-MAR-2009 Journal Article - POSTPRINT 01-MAR-2008 -- 01-MAR-2009 Lysozyme -Mediated Formation of Protein–Silica Nano-Composites for

  17. 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

    2011-06-03

    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.

  18. Development and evaluation of fast forming nano-composite hydrogel for ocular delivery of diclofenac.

    PubMed

    Li, Xingyi; Zhang, Zhaoliang; Chen, Hao

    2013-05-01

    In this paper, a fast forming nano-composite hydrogel was developed for potential application in ocular drug delivery. The optical transmission (OT) as well as rheological properties of nano-composite hydrogel was characterized. The developed nano-composite hydrogel given a high diclofenac micelles loading and provided a sustained release manner of diclofenac within 6h. The developed nano-composite hydrogel formulation was administrated into the eye as flowable solution, quickly forming a hydrogel that is able to resist of the blinking and flushing of tear, yet resulting in the prolonged residence time of pre-corneal. In vivo eye irritation test suggested that the developed nano-composite hydrogel was none-eye irritation might be suitable for various ocular applications. In vivo pharmacokinetic study indicated that the developed nano-composite hydrogel could significantly increase the bioavailability of diclofenac and maintain the concentration of diclofenac in aqueous humor above MEC at least 24h after administration as compared with that of the commercial diclofenac sodium eye drops, which might be able to reduce the frequency of administration for patients.

  19. Damping Behavior of Alumina Epoxy Nano-Composites

    NASA Astrophysics Data System (ADS)

    Katiyar, Priyanka; Kumar, Anand

    2016-10-01

    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. Effect of water vapors on the luminescence of cation-exchange membranes modified by Pt(II) and Ru(II) complexes and Nile blue

    NASA Astrophysics Data System (ADS)

    Khakhalina, M. S.; Musaeva, D. N.; Tikhomirova, I. Yu.; Puzyk, M. V.

    2010-04-01

    The surface of a cation-exchange membrane was modified by the [PtEnPpy]+, [PtEnBt]+, [PtEnTpy]+, [RuBpy3]+2, and NB+, (En is ethylenediamine; Ppy, Bt, Tpy are α-deprotonated forms of 2-phenylpyridine, 2-phenylbenzothiazole, and 2-(2'-thienyl)pyridine, respectively; Bpy is 2,2'-bipyridyl, and NB+ is Nile blue) ions, which exhibit intense luminescence. It is found that the quenching of the luminescence of the modified cation-exchange membrane by water vapors depends on the nature of the excited electronic state of the immobilized cation.

  1. 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.

  2. Simple and novel electrochemical sensor for the determination of tetracycline based on iron/zinc cations-exchanged montmorillonite catalyst.

    PubMed

    Gan, Tian; Shi, Zhaoxia; Sun, Junyong; Liu, Yanming

    2014-04-01

    A simple and novel electrochemical sensor for the determination of tetracycline (TC), a kind of antibiotic that may induce residue in the food chain, was developed by the modification of iron/zinc cation-exchanged montmorillonite (Fe/Zn-MMT) catalyst on glassy carbon electrode (GCE). The morphology and the structure of the Fe/Zn-MMT nanomaterial were characterized by scanning electron microscopy and X-ray diffraction, respectively. The results of electrochemical experiments demonstrated that the sensor exhibited excellent electrocatalytic activity to the oxidation of TC in the presence of sodium dodecyl sulfate. The sensor displayed a wide linear range from 0.30 to 52.0 μM and a low detection limit of 0.10 μM by using the derivative differential pulse voltammetry. Moreover, the electrochemical sensor was applied to the detection of TC in feedstuff and meat samples.

  3. 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.

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

    DOE PAGES

    Pezeshki, Alan M.; Fujimoto, Cy; Sun, Che -Nan; ...

    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

  5. Perfluorinated carbon-chain copolymers with functional groups and cation exchange membranes based on them: synthesis, structure and properties

    NASA Astrophysics Data System (ADS)

    Kirsh, Yu E.; Smirnov, S. A.; Popkov, Yu M.; Timashev, Sergei F.

    1990-06-01

    The review is devoted to perfluorinated polymers with sulphonic and carboxylic acid groups and to cation exchange membranes based on them. The synthesis is described of copolymers of tetrafluoroethylene with perfluorovinyl ethers containing functional groups by radical copolymerisation in an organic medium and in aqueous emulsions. Special features of the copolymerisation and approaches to obtaining copolymers with set characteristics are discussed. Data are presented on the structure and physicochemical properties of the polymeric films. Attempts to form membranes from the polymers obtained, the means of strengthening them and methods for chemical modification are described. Data are correlated on the influence of structure and polymer composition and the nature of the functional groups on the electrochemical characteristics of membranes. Special features of the functioning of perfluorinated membranes in the process for making chlorine and alkali by the electrolysis of sodium chloride solution are considered. The bibliography has 104 references.

  6. 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

  7. 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

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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.

  13. 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.

  14. 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...

  15. 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

    2012-04-06

    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.

  16. Evaluation of strong cation-exchange polymers for the determination of drugs by solid-phase extraction-liquid chromatography-tandem mass spectrometry.

    PubMed

    Fontanals, Núria; Miralles, Núria; Abdullah, Norhayati; Davies, Arlene; Gilart, Núria; Cormack, P A G

    2014-05-23

    This paper presents eight distinct strong cation-exchange resins, all of which were derived from precursor resins that had been synthesised using either precipitation polymerisation or non-aqueous dispersion polymerisation. The precursor resins were transformed into the corresponding strong cation-exchange resins by hypercrosslinking followed by polymer analogous reactions, to yield materials with high specific surface areas and strong cation-exchange character. These novel resins were then evaluated as strong cation-exchange (SCX) sorbents in the solid-phase extraction (SPE) of a group of drugs from aqueous samples. Following preliminary experiments, the two best-performing resins were then evaluated in solid-phase extraction-liquid chromatography-tandem mass spectrometry (SPE/LC-MS/MS) to determine a group of drugs from sewage samples. In general, use of these sorbents led to excellent recovery values (75-100%) for most of the target drugs and negligible matrix effects (ME) (<20% ion suppression/enhancement of the analyte signal), when 50mL and 25mL of effluent and influent sewage water samples, respectively, were percolated through the resins. Finally, a validated method based on SPE/LC-MS/MS was used to quantify the target drugs present in different sewage samples.

  17. Sorption of doubly charged metal ions from MeF/sub 2/-HF(NH/sub 4/FHF)-H/sub 2/O solutions by KFP-12 cation-exchange resin

    SciTech Connect

    Ganyaev, V.P.; Pimneva, L.A.; Pakholkov, V.S.; Andrianova, L.I.; Topalova, O.V.

    1982-06-20

    This report is a continuation of studies of ion exchange on various cation-exchangers. Experimental and calculated data on sorption of copper(II), zinc, cadmium, mercury, beryllium, manganese(II), cobalt, and nickel cations from solutions of hydrofluoric acid and ammonium hydrogen fluoride by the macroporous phosphate cation-exchange resin KFP-12 are examined.

  18. 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.

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

    PubMed

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

    2008-01-01

    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.

  20. Role of tentacles and protein loading on pore accessibility and mass transfer in cation exchange materials for proteins.

    PubMed

    Thomas, Helen; Coquebert de Neuville, Bertrand; Storti, Giuseppe; Morbidelli, Massimo; Joehnck, Matthias; Schulte, Michael

    2013-04-12

    In protein chromatography, the size of the protein determines which fraction of pores it can access within a resin and at which rate of diffusion. Moreover, in the presence of grafted polymers like in advanced materials, adsorbed proteins and electrolytes complicate the interaction pore-protein. In this study, we evaluated in a comparative way the behavior of Fractogel EMD SO3 (M) and (S), "tentacle"-type, strong cation exchangers, as well as a reference material without tentacles, all of which are commonly used for protein purification. ISEC experiments were carried out with a set of Dextran tracers of largely different molecular size covering the typical range of protein sizes. Experimental values of porosity (internal and external to the particles) as well as of pore diffusion coefficients have been measured at different NaCl concentrations and under protein loading. These results provide useful insights into the complex interplay among mentioned factors: first, the presence of tentacles induces size exclusion selectivity in the materials; second, the salt induces conformational changes of the tentacles, leading to porosities larger than expected in tentacle materials; third, protein adsorption mainly leads to a reduction of porosity due to pore space occupied by the protein and to a decrease of pore diffusion coefficient.

  1. Solid cation exchange phase to remove interfering anthocyanins in the analysis of other bioactive phenols in red wine.

    PubMed

    da Silva, Letícia Flores; Guerra, Celito Crivellaro; Klein, Diandra; Bergold, Ana Maria

    2017-07-15

    Bioactive phenols (BPs) are often targets in red wine analysis. However, other compounds interfere in the liquid chromatography methods used for this analysis. Here, purification procedures were tested to eliminate anthocyanin interference during the determination of 19 red-wine BPs. Liquid chromatography, coupled to a diode array detector (HPLC-DAD) and a mass spectrometer (UPLC-MS), was used to compare the direct injection of the samples with solid-phase extractions: reversed-phase (C18) and strong cation-exchange (SCX). The HPLC-DAD method revealed that, out of 13BPs, only six are selectively analyzed with or without C18 treatment, whereas SCX enabled the detection of all BPs. The recovery with SCX was above 86.6% for eight BPs. Moreover, UPLC-MS demonstrated the potential of SCX sample preparation for the determination of 19BPs. The developed procedure may be extended to the analysis of other red wine molecules or to other analytical methods where anthocyanins may interfere.

  2. Immobilization of polyethylenimine nanoclusters onto a cation exchange resin through self-crosslinking for selective Cu(II) removal.

    PubMed

    Chen, Yiliang; Pan, Bingcai; Zhang, Shujuan; Li, Haiyan; Lv, Lu; Zhang, Weiming

    2011-06-15

    Donnan membrane principle provides great opportunities for development of highly efficient adsorbents for toxic metals abatement. Based on the principle we prepared a new composite adsorbent by immobilizing polyethylenimine (PEI) nanoclusters within a macroporous cation exchanger D001 through self-crosslinking by glutaraldehyde upon Cu(II)-template process. Negligible PEI loss was observed from the resultant composite adsorbent D001-PEI-GA to solution of pHs 1-12. Increasing solution pH from 1 to 6 results in more favorable Cu(II) retention by D001-PEI-GA, and Cu(II) adsorption onto D001-PEI-GA follows the pseudo-second-order kinetic model well. Compared to D001, D001-PEI-GA displays more preferable Cu(II) sequestration in the presence of co-ions Mg(2+), Ca(2+), Sr(2+) at higher levels. Fixed-bed adsorption of a synthetic solution containing Cu(II) and other co-ions showed that Cu(II) sequestration on D001-PEI-GA could result in its conspicuous decrease from 5mg/L to below 0.01 mg/L with the treatment volume as high as 630 BV per run, while that for D001 was only ∼ 85 BV. Also, the spent composite adsorbent can be readily regenerated by HCl (0.3M)-NaCl (0.5M) binary solution for repeated use with negligible capacity loss.

  3. 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.

  4. Kinetics, thermodynamics and surface heterogeneity assessment of uranium(VI) adsorption onto cation exchange resin derived from a lignocellulosic residue

    NASA Astrophysics Data System (ADS)

    Anirudhan, T. S.; Radhakrishnan, P. G.

    2009-02-01

    A new cation exchange resin (PGTFS-COOH) having a carboxylate functional group at the chain end was prepared by grafting poly(hydroxyethylmethacrylate) onto tamarind fruit shell, TFS (a lignocellulosic residue) using potassium peroxydisulphate-sodium thiosulphate redox initiator, and in the presence of N,N'-methylenebisacrylamide (MBA) as a crosslinking agent, followed by functionalisation. The adsorbent was characterized with the help of FTIR, XRD, scanning electron micrographs (SEM), and potentiometric titrations. The kinetic and isotherm data, obtained at optimum pH value 6.0 at different temperatures could be fitted with pseudo-second-order equation and Sips isotherm model, respectively. An increase in temperature induces positive effect on the adsorption process. The calculated activation energy of adsorption ( Ea, 18.67 kJ/mol) indicates that U(VI) adsorption was largely due to diffusion-controlled process. The values of adsorption enthalpy, Gibbs free energy, and entropy were calculated using thermodynamic function relationships. The decrease in adsorption enthalpy with increasing U(VI) uploading on the adsorbent, reflects the surface energetic heterogeneity of the adsorbent. The isosteric heat of adsorption was quantitatively correlated with the fractional loading for the U(VI) ions adsorption onto PGTFS-COOH. The results showed that the PGTFS-COOH possessed heterogeneous surface with sorption sites having different activities.

  5. Comparison between methods using copper, lanthanum, and colorimetry for the determination of the cation exchange capacity of plant cell walls.

    PubMed

    Wehr, J Bernhard; Blamey, F Pax C; Menzies, Neal W

    2010-04-28

    The determination of the cation exchange capacity (CEC) of plant cell walls is important for many physiological studies. We describe the determination of cell wall CEC by cation binding, using either copper (Cu) or lanthanum (La) ions, and by colorimetry. Both cations are strongly bound by cell walls, permitting fast and reproducible determinations of the CEC of small samples. However, the dye binding methods using two cationic dyes, Methylene Blue and Toluidine Blue, overestimated the CEC several-fold. Column and centrifugation methods are proposed for CEC determination by Cu or La binding; both provide similar results. The column method involves packing plant material (2-10 mg dry mass) in a chromatography column (10 mL) and percolating with 20 bed volumes of 1 mM La or Cu solution, followed by washing with deionized water. The centrifugation method uses a suspension of plant material (1-2 mL) that is centrifuged, and the pellet is mixed three times with 10 pellet volumes of 1 mM La or Cu solution followed by centrifugation and final washing with deionized water. In both methods the amount of La or Cu bound to the material was determined by spectroscopic methods.

  6. 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.

  7. 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.

  8. Competition and enhancement effect in coremoval of atenolol and copper by an easily regenerative magnetic cation exchange resin.

    PubMed

    Li, Qimeng; Wang, Zheng; Li, Qiang; Shuang, Chendong; Zhou, Qing; Li, Aimin; Gao, Canzhu

    2017-03-06

    This paper aimed to investigate the removal of combined Cu(2+) and atenolol (ATL) in aqueous solution by using a newly synthesized magnetic cation exchange resin (MCER) as the adsorbent. The MCER exhibited efficient removal performance in sole, binary, pre-loading and saline systems. The adsorption kinetics of Cu(2+) and ATL fitted both pseudo-first-order and pseudo-second order model, while better described by pseudo-second order model in binary system. In mixed Cu(2+) and ATL solution, the adsorption of ATL was suppressed due to direct competition of carboxylic groups, while Cu(2+) adsorption was enhanced because of the formation of surface complexes. This increasing in heterogeneity was demonstrated by adsorption isotherms, which were more suitable for Freundlich model in binary system, while better described by Langmuir model in sole system. As proved by FTIR and XPS spectra, both amino and hydroxyl groups of ATL could form complexes with Cu(2+). Decomplexing-bridging interaction was elucidated as the leading mechanism in coremoval of Cu(2+) and ATL, which involved [Cu-ATL] decomplexing and newly created Cu- or ATL sites for additional bridging. For saline system, the resulting competition and enhancement effects in mixed solution were amplified with the addition of co-existing cations. Moreover, the MCER could be effectively regenerated by 0.01 M HCl solution and maintain high stability over 5 adsorption-desorption cycles, which render it great potential for practical applications.

  9. Advanced analytical method of nereistoxin using mixed-mode cationic exchange solid-phase extraction and GC/MS.

    PubMed

    Park, Yujin; Choe, Sanggil; Lee, Heesang; Jo, Jiyeong; Park, Yonghoon; Kim, Eunmi; Pyo, Jaesung; Jung, Jee H

    2015-07-01

    Nereistoxin(NTX) was originated from a marine annelid worm Lumbriconereis heteropoda and its analogue pesticides including cartap, bensultap, thiocyclam and thiobensultap have been commonly used in agriculture, because of their low toxicity and high insecticidal activity. However, NTX has been reported about its inhibitory neuro toxicity in human and animal body, by blocking nicotinic acetylcholine receptor and it cause significant neuromuscular toxicity, resulting in respiratory failure. We developed a new method to determine NTX in biological fluid. The method involves mixed-mode cationic exchange based solid phase extraction and gas chromatography/mass spectrometry for final identification and quantitative analysis. The limit of detection and recovery were substantially better than those of other methods using liquid-liquid extraction or headspace solid phase microextraction. The good recoveries (97±14%) in blood samples were obtained and calibration curves over the range 0.05-20 mg/L have R2 values greater than 0.99. The developed method was applied to a fatal case of cartap intoxication of 74 years old woman who ingested cartap hydrochloride for suicide. Cartap and NTX were detected from postmortem specimens and the cause of the death was ruled to be nereistoxin intoxication. The concentrations of NTX were 2.58 mg/L, 3.36 mg/L and 1479.7 mg/L in heart, femoral blood and stomach liquid content, respectively. The heart blood/femoral blood ratio of NTX was 0.76.

  10. Selective Cu{sup 2+} and Pb{sup 2+} exchange with highly charged cation exchanger of Na-4-mica

    SciTech Connect

    Kodama, Tatsuya; Komarneni, Sridhar

    1999-09-01

    Selective cation exchange for Cu and Pb has been demonstrated with the high-charge-density sodium fluorophlogopite mica, Na-4-mica. The 2Na{sup +} {yields} M{sup 2+} exchange reaction (M = Cu or Pb) was investigated with Na-4-micas prepared by two different synthetic processes. One was easily and economically prepared by crystallization from a mixture of NaF, MgO, and metakaolin, the latter serves as an inexpensive aluminosilicate source. Another was prepared by solution-sol-gel processing. Ion-exchange isotherms for Cu{sup 2+} and Pb{sup 2+} were obtained at room temperature. The thermodynamic functions for the initial ion-exchange reactions were calculated because the isotherms were not completed., High selectivities for both copper and lead exchange were found on the highly crystallized Na-4-mica prepared from metakaolin. Their ion-exchange capacities were 225 and 257 milliequivalents per 100 g of dry clay for Cu{sup 2+} and Pb{sup 2+}, respectively. This high level decontamination of copper and lead with the highly crystallized Na-4-mica from metakaolin will be a very important separation required for purification of drinking water as well as for wastewater treatment and disposal.

  11. The influence of organic sample solvents on the separation efficiency of basic compounds under strong cation exchange mode.

    PubMed

    Long, Zhen; Yu, Dongping; Liu, Yanfang; Du, Nana; Tao, Yanduo; Mei, Lijuan; Guo, Zhimou; Liang, Xinmiao

    2015-05-04

    This study investigated the influence of organic sample solvents on separation efficiency of basic compounds under strong cation exchange (SCX) mode. The mixtures of acidic aqueous solution and organic solvent such as acetonitrile, ethanol, methanol and dimethyl sulfoxide (DMSO) were tested as sample solvents. For later-eluting analytes, the increase of sample solvent elution strength was responsible for the decrease of separation efficiency. Thus, sample solvents with weak elution strength could provide high separation efficiencies. For earlier-eluting analytes, the retention of organic sample solvents was the main factor affecting separation efficiency. Weakly retained solvents could provide high separation efficiency. In addition, an optimized approach was proposed to reduce the effect of organic sample solvent, in which low ionic solvent was employed as initial mobile phase in the gradient. At last, the analysis of impurities in hydrophobic drug berberine was performed. The results showed that using acidic aqueous methanol as sample solvents could provide high separation efficiency and good resolution (R>1.5).

  12. Effect of magnesium/calcium ratio in solutions subjected to electrodialysis: characterization of cation-exchange membrane fouling.

    PubMed

    Casademont, Christophe; Pourcelly, Gérald; Bazinet, Laurent

    2007-11-15

    Electrodialysis is based on the migration of charged species through perm-selective membranes under an electric field. Fouling, which is the accumulation of undesired solid materials at the interfaces of these membranes, is one of the major problems of this process. The aim of the present work was to investigate the nature and the morphology of fouling observed at different Mg/Ca ratios (R=0, 1/20, 1/10, 1/5, 2/5) on cation-exchange membranes (CEM) during conventional electrodialysis treatments. It appeared that for R=0, the fouling observed on the surface in contact with the basified concentrate was formed of only Ca(OH)2. As soon as magnesium was introduced into the solution treated, CaCO3 was observed. Furthermore, the X-ray diffraction results also identified the CaCO3 observed as calcite. To our knowledge, this is the first time that the presence of magnesium has been demonstrated to induce a CaCO3 fouling on CEM during electrodialysis.

  13. Comparing the short and long term stability of biodegradable, ceramic and cation exchange membranes in microbial fuel cells.

    PubMed

    Winfield, Jonathan; Chambers, Lily D; Rossiter, Jonathan; Ieropoulos, Ioannis

    2013-11-01

    The long and short-term stability of two porous dependent ion exchange materials; starch-based compostable bags (BioBag) and ceramic, were compared to commercially available cation exchange membrane (CEM) in microbial fuel cells. Using bi-directional polarisation methods, CEM exhibited power overshoot during the forward sweep followed by significant power decline over the reverse sweep (38%). The porous membranes displayed no power overshoot with comparably smaller drops in power during the reverse sweep (ceramic 8%, BioBag 5.5%). The total internal resistance at maximum power increased by 64% for CEM compared to 4% (ceramic) and 6% (BioBag). Under fixed external resistive loads, CEM exhibited steeper pH reductions than the porous membranes. Despite its limited lifetime, the BioBag proved an efficient material for a stable microbial environment until failing after 8 months, due to natural degradation. These findings highlight porous separators as ideal candidates for advancing MFC technology in terms of cost and operation stability.

  14. 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.

  15. 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

    2017-04-01

    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.

  16. 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.

  17. Dynamics of the separation of amino acid and mineral salt in the stationary dialysis of solutions with an MK-40 profiled sulfo group cation exchange membrane

    NASA Astrophysics Data System (ADS)

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

    2012-11-01

    The conjugated diffusion transport of amino acid and mineral salt through a profiled sulfo group cation exchange membrane that simulates the extraction of amino acid from wash waters of microbiological production containing mineral components not used in synthesis is studied. The competitive nature of the conjugation of flows resulting in a decrease in the rate of the mass transfer of components and their separation factor is established from a comparative analysis of experimental data on the diffusion transfer of phenylalanine and sodium chloride in the form of hydrogen from individual and mixed solutions through a profiled sulfo group cation exchange membrane. The range of concentrations and the ratio of components in solution corresponding to the effective separation of phenylalanine and sodium chloride are determined.

  18. 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).

  19. 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

  20. Synthesis and characterization of a new inorganic cation-exchanger-Zr(IV) tungstomolybdate: analytical applications for metal content determination in real sample and synthetic mixture.

    PubMed

    Nabi, Syed Ashfaq; Naushad, Mu; Inamuddin

    2007-04-02

    An amorphous sample of inorganic cation-exchanger Zr(IV) tungstomolybdate was prepared by mixing varying ratios of 0.1M aqueous solution of sodium tungstate and 0.1M aqueous solution of sodium molybdate into 0.1M aqueous solution of zirconium oxychloride at pH 1. This cation-exchanger was found to have a good ion-exchange capacity (2.40 mequiv.g(-1) for Na(+)), high thermal and chemical stability. A tentative structural formula was proposed on the basis of chemical composition, FTIR and thermogravimetric analysis. Distribution coefficients (K(d)) values of metal ions in various solvent systems were determined. Some important and analytically difficult quantitative binary separations viz. Ni(II)-Pb(II), Ni(II)-Zn(II), Ni(II)-Cd(II), Mg(II)-Al(III), etc. were achieved. The practical applicability of the cation-exchanger was demonstrated in the separation of Cu(II)-Zn(II) from a synthetic mixture as well as from real samples of pharmaceutical formulation and brass alloy.

  1. 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.

  2. 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.

  3. 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.

  4. [Preparation of weak cation exchange monolithic column and its applications for on-line determination of nifedipine in human plasma].

    PubMed

    Yang, Xinru; Yang, Gengliang; Zhu, Tao; Feng, Xiaojuan; Yang, Guanqun

    2009-03-01

    A cation exchange monolithic column was prepared with methylacrylic acid (MAA) as the functional monomer and ethylene dimethacrylate (EDMA) as the cross linker. This column was applied to remove the matrix compounds and enrich the ionic medicines in human plasma with water as the mobile phase. As a result, the human plasma samples can be directly injected into chromatographic system. The relationship between the mobile phase flow rate and back pressure was studied. The results showed that the monolithic column had good performances in lower pressure and higher permeability. In addition, the maximum adsorption of nifedipine on this monolithic column was investigated. The on-line clean-up and enrichment of samples were carried out using this column as the solid-phase extraction material and the C18 column as the analytical column. The chromatography was performed on a C18 reversed-phase high performance liquid chromatographic column with ultraviolet detection at 235 nm. The mobile phase was a mixture of methanol-water (70:30, v/v), and the flow rate was 1.0 mL/min. The linear range of nifedipine in human plasma was 5.0-75.0 microg/L. The intra- and inter-day relative standard deviations (RSDs) were both less than 5.0%. The limit of detection (LOD) was 1 microg/L and the limit of quantification (LOQ) was 4 microg/L. In this method tedious pretreatment procedure is not necessary. It is a fast, economical, reproducible and efficient method for assaying trace nifedipine in human plasma.

  5. Strong cation exchange-type chiral stationary phase for enantioseparation of chiral amines in subcritical fluid chromatography.

    PubMed

    Wolrab, Denise; Kohout, Michal; Boras, Mario; Lindner, Wolfgang

    2013-05-10

    A new strong cation exchange type chiral stationary phase (SCX CSP) based on a syringic acid amide derivative of trans-(R, R)-2-aminocyclohexanesulfonic acid was applied to subcritical fluid chromatography (SFC) for separation of various chiral basic drugs and their analogues. Mobile phase systems consisting of aliphatic alcohols as polar modifiers and a broad range of amines with different substitution patterns and lipophilicity were employed to evaluate the impact on the SFC retention and selectivity characteristics. The observed results point to the existence of carbonic and carbamic acid salts formed as a consequence of reactions occurring between carbon dioxide, the alcoholic modifiers and the amine species present in the sub/supercritical fluid medium, respectively. Evidence is provided that these species are essential for affecting ion exchange between the strongly acidic chiral selector units and the basic analytes, following the well-established stoichiometric displacement mechanisms. Specific trends were observed when different types of amines were used as basic additives. While ammonia gave rise to the formation of the most strongly eluting carbonic and carbamic salt species, simple tertiary amines consistently provided superior levels of enantioselectivity. Furthermore, trends in the chiral SFC separation characteristics were investigated by the systematic variation of the modifier content and temperature. Different effects of additives are interpreted in terms of changes in the relative concentration of the transient ionic species contributing to analyte elution, with ammonia-derived carbamic salts being depleted at elevated temperatures by decomposition. Additionally, in an effort to optimize SFC enantiomer separation conditions for selected analytes, the impact of the type of the organic modifier, temperature, flow rate and active back pressure were also investigated.

  6. 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.

  7. Analysis of ustiloxins in rice using polymer cation exchange cleanup followed by liquid chromatography-tandem mass spectrometry.

    PubMed

    Cao, Zhao-Yun; Sun, Li-Hua; Mou, Ren-Xiang; Lin, Xiao-Yan; Zhou, Rong; Ma, You-Ning; Chen, Ming-Xue

    2016-12-09

    Ustiloxins are cyclopeptide mycotoxins produced by the pathogenic fungus Ustilaginoidea virens of rice false smut. Quantification of ustiloxins is essential to assess the food safety of rice infected by rice false smut disease. This paper describes a sensitive method for the simultaneous quantification of ustiloxins A, B, C, D and F in rice grains using liquid chromatography-tandem mass spectrometry (LC-MS/MS). Since notable matrix enhancement effects (21%-78%) occurred for all of the target analytes (except for ustiloxin A), several solid phase extraction materials were tested for their ability to retain ustiloxins from aqueous solutions prior to the LC-MS/MS analysis, including C18 sorbents, polymer anion exchange sorbents resin (PAX), and polymer cation exchange resin (PCX). The PCX resin was adopted due to its higher extraction capability and selectivity for all targets compared to others, and in this case, almost no matrix effects (-5% to 8%) were observed for all of the ustiloxins monitored. The developed method reached limits of quantification of 0.2-2ngg(-1), and linearity was statistically verified over two orders of magnitude with regression coefficients (R(2))>0.991. The mean recoveries were from 85% to 109%, and the inter-day precisions (n=11) were less than 16%, with intra-day precisions (n=6) within 12%. Analysis of samples showed that ustiloxin A was the dominant species, with the content ranging from 5.5 to 273.8ngg(-1), followed by ustiloxin B (≤88.7ngg(-1)), while concentrations of ustiloxins C, D and F were slightly lower (≤43.2ngg(-1)). To our knowledge, this is the first report on the determination and analysis of five ustiloxins simultaneously in a single analysis.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. Orientated Nano-Composites: Relationships Between Nano-Structure and Mechanical Properties

    DTIC Science & Technology

    2004-11-01

    reviewing instructions, searching existing data sources, gathering and maintaining the data needed, and completing and reviewing the collection of...a range of modifiers, including organoclays , silica nanoparticles and carbon nanotubes. The mechanical and fracture properties of these materials have...Std Z39-18 2 Abstract Epoxy nano-composites have been manufactured using a range of modifiers, including organoclays , silica nanoparticles and

  13. 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

  14. 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

    2016-08-05

    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.

  15. Polypyrrole based gas sensor for ammonia detection

    NASA Astrophysics Data System (ADS)

    Dunst, K. J.; Cysewska, K.; Kalinowski, P.; Jasiński, P.

    2016-01-01

    The nature of polypyrrole response to toxic gases does not allow using the sensor in a conventional way. The main aim of this study is to acquire the information about the concentration using different approaches: a linear approximation, a non-linear approximation and a tangent method. In this paper a two-steps procedure for sensor response measurements has been utilized. Polypyrrole films were electrochemically synthesized on the interdigitated electrodes. Gas sensing measurements of polypyrrole based sensor were carried out at room temperature. The influence of the flow rate on the sensing performance to NH3 were investigated. The preliminary studies of aging of the sensor were also explored.

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

    PubMed

    Guo, Jing; Carta, Giorgio

    2015-04-03

    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

  18. Preparation of a novel dual-function strong cation exchange/hydrophobic interaction chromatography stationary phase for protein separation.

    PubMed

    Zhao, Kailou; Yang, Li; Wang, Xuejiao; Bai, Quan; Yang, Fan; Wang, Fei

    2012-08-30

    We have explored a novel dual-function stationary phase which combines both strong cation exchange (SCX) and hydrophobic interaction chromatography (HIC) characteristics. The novel dual-function stationary phase is based on porous and spherical silica gel functionalized with ligand containing sulfonic and benzyl groups capable of electrostatic and hydrophobic interaction functionalities, which displays HIC character in a high salt concentration, and IEC character in a low salt concentration in mobile phase employed. As a result, it can be employed to separate proteins with SCX and HIC modes, respectively. The resolution and selectivity of the dual-function stationary phase were evaluated under both HIC and SCX modes with standard proteins and can be comparable to that of conventional IEC and HIC columns. More than 96% of mass and bioactivity recoveries of proteins can be achieved in both HIC and SCX modes, respectively. The results indicated that the novel dual-function column could replace two individual SCX and HIC columns for protein separation. Mixed retention mechanism of proteins on this dual-function column based on stoichiometric displacement theory (SDT) in LC was investigated to find the optimal balance of the magnitude of electrostatic and hydrophobic interactions between protein and the ligand on the silica surface in order to obtain high resolution and selectivity for protein separation. In addition, the effects of the hydrophobicity of the ligand of the dual-function packings and pH of the mobile phase used on protein separation were also investigated in detail. The results show that the ligand with suitable hydrophobicity to match the electrostatic interaction is very important to prepare the dual-function stationary phase, and a better resolution and selectivity can be obtained at pH 6.5 in SCX mode. Therefore, the dual-function column can replace two individual SCX and HIC columns for protein separation and be used to set up two-dimensional liquid

  19. 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

  20. 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.

  1. 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.

  2. Exchange bias and anisotropy analysis of nano-composite Co84Zr16N thin films

    NASA Astrophysics Data System (ADS)

    Singh, Jitendra; Taube, William Ringal; Ansari, Akhtar Saleem; Gupta, Sanjeev Kumar; Kulriya, Pawan Kumar; Akhtar, Jamil

    2015-03-01

    Nano-composite Co84Zr16N (CZN) films were prepared by reactive co-sputter deposition. As-deposited CZN films have not shown any exchange bias effect. But annealed (390 K) and field cooled samples have shown exchange bias phenomena. The observed exchange bias is attributed to inter-cluster exchange coupling between ferromagnetic and antiferromagnetic nano-composite phase. High resolution transmission electron microscope study reveals that, the CZN films are composed of ordered and crystalline ferromagnetic Cobalt nano-clusters embedded in an antiferromagnetic matrix. X-ray diffraction confirms the poly-crystalline growth of the CZN films with a preferred fcc (622) phase formation. In-plane anisotropy of the exchange biased films was investigated by rotational magnetization curve, and the analysis shows that the magnetization reversal behaves according to the coherent rotation of the magnetic moment vector. Effectively, exchange bias effect in such single layer films could be attributed to co-existing antiferromagnetic and ferromagnetic phase within the single layer. Such single layer nano-composite films can be a possible alternative to the bilayer combination of antiferromagnetic/ferromagnetic exchange biased films and are ideally suited for spintronics and tunnel junction applications.

  3. Highly Emissive Divalent-Ion-Doped Colloidal CsPb1-xMxBr3 Perovskite Nanocrystals through Cation Exchange.

    PubMed

    van der Stam, Ward; Geuchies, Jaco J; Altantzis, Thomas; van den Bos, Karel H W; Meeldijk, Johannes D; Van Aert, Sandra; Bals, Sara; Vanmaekelbergh, Daniel; de Mello Donega, Celso

    2017-03-22

    Colloidal CsPbX3 (X = Br, Cl, and I) perovskite nanocrystals (NCs) have emerged as promising phosphors and solar cell materials due to their remarkable optoelectronic properties. These properties can be tailored by not only controlling the size and shape of the NCs but also postsynthetic composition tuning through topotactic anion exchange. In contrast, property control by cation exchange is still underdeveloped for colloidal CsPbX3 NCs. Here, we present a method that allows partial cation exchange in colloidal CsPbBr3 NCs, whereby Pb(2+) is exchanged for several isovalent cations, resulting in doped CsPb1-xMxBr3 NCs (M= Sn(2+), Cd(2+), and Zn(2+); 0 < x ≤ 0.1), with preservation of the original NC shape. The size of the parent NCs is also preserved in the product NCs, apart from a small (few %) contraction of the unit cells upon incorporation of the guest cations. The partial Pb(2+) for M(2+) exchange leads to a blue-shift of the optical spectra, while maintaining the high photoluminescence quantum yields (>50%), sharp absorption features, and narrow emission of the parent CsPbBr3 NCs. The blue-shift in the optical spectra is attributed to the lattice contraction that accompanies the Pb(2+) for M(2+) cation exchange and is observed to scale linearly with the lattice contraction. This work opens up new possibilities to engineer the properties of halide perovskite NCs, which to date are demonstrated to be the only known system where cation and anion exchange reactions can be sequentially combined while preserving the original NC shape, resulting in compositionally diverse perovskite NCs.

  4. Highly Emissive Divalent-Ion-Doped Colloidal CsPb1–xMxBr3 Perovskite Nanocrystals through Cation Exchange

    PubMed Central

    2017-01-01

    Colloidal CsPbX3 (X = Br, Cl, and I) perovskite nanocrystals (NCs) have emerged as promising phosphors and solar cell materials due to their remarkable optoelectronic properties. These properties can be tailored by not only controlling the size and shape of the NCs but also postsynthetic composition tuning through topotactic anion exchange. In contrast, property control by cation exchange is still underdeveloped for colloidal CsPbX3 NCs. Here, we present a method that allows partial cation exchange in colloidal CsPbBr3 NCs, whereby Pb2+ is exchanged for several isovalent cations, resulting in doped CsPb1–xMxBr3 NCs (M= Sn2+, Cd2+, and Zn2+; 0 < x ≤ 0.1), with preservation of the original NC shape. The size of the parent NCs is also preserved in the product NCs, apart from a small (few %) contraction of the unit cells upon incorporation of the guest cations. The partial Pb2+ for M2+ exchange leads to a blue-shift of the optical spectra, while maintaining the high photoluminescence quantum yields (>50%), sharp absorption features, and narrow emission of the parent CsPbBr3 NCs. The blue-shift in the optical spectra is attributed to the lattice contraction that accompanies the Pb2+ for M2+ cation exchange and is observed to scale linearly with the lattice contraction. This work opens up new possibilities to engineer the properties of halide perovskite NCs, which to date are demonstrated to be the only known system where cation and anion exchange reactions can be sequentially combined while preserving the original NC shape, resulting in compositionally diverse perovskite NCs. PMID:28260380

  5. Variation in whole DNA methylation in red maple (Acer rubrum) populations from a mining region: association with metal contamination and cation exchange capacity (CEC) in podzolic soils.

    PubMed

    Kalubi, K N; Mehes-Smith, M; Spiers, G; Omri, A

    2017-02-15

    Although a number of publications have provided convincing evidence that abiotic stresses such as drought and high salinity are involved in DNA methylation reports on the effects of metal contamination, pH, and cation exchange on DNA modifications are limited. The main objective of the present study is to determine the relationship between metal contamination and Cation exchange capacity (CEC) on whole DNA modifications. Metal analysis confirms that nickel and copper are the main contaminants in sampled sites within the Greater Sudbury Region (Ontario, Canada) and liming has increased soil pH significantly even after 30 years following dolomitic limestone applications. The estimated CEC values varied significantly among sites, ranging between 1.8 and 10.5 cmol(+) kg(-1), with a strong relationship being observed between CEC and pH (r = 0.96**). Cation exchange capacity, significantly lower in highly metal contaminated sites compared to both reference and less contaminated sites, was higher in the higher organic matter limed compared to unlimed sites. There was a significant variation in the level of cytosine methylation among the metal-contaminated sites. Significant and strong negative correlations between [5mdC]/[dG] and bioavailable nickel (r = -0.71**) or copper (r = -0.72**) contents were observed. The analysis of genomic DNA for adenine methylation in this study showed a very low level of [6N-mdA]/dT] in Acer rubrum plants analyzed ranging from 0 to 0.08%. Significant and very strong positive correlation was observed between [6N-mdA]/dT] and soil bioavailable nickel (r = 0.78**) and copper (r = 0.88**) content. This suggests that the increased bioavailable metal levels associated with contamination by nickel and copper particulates are associated with cytosine and adenine methylation.

  6. Separation of aliphatic carboxylic acids and benzenecarboxylic acids by ion-exclusion chromatography with various cation-exchange resin columns and sulfuric acid as eluent.

    PubMed

    Ohta, Kazutoku; Ohashi, Masayoshi; Jin, Ji-Ye; Takeuchi, Toyohide; Fujimoto, Chuzo; Choi, Seong-Ho; Ryoo, Jae-Jeong; Lee, Kwang-Pill

    2003-05-16

    The application of various hydrophilic cation-exchange resins for high-performance liquid chromatography (sulfonated silica gel: TSKgel SP-2SW, carboxylated silica gel: TSKgel CM-2SW, sulfonated polymethacrylate resin: TSKgel SP-5PW, carboxylated polymethacrylate resins: TSKgel CM-5PW and TSKgel OA-Pak A) as stationary phases in ion-exclusion chromatography for C1-C7 aliphatic carboxylic acids (formic, acetic, propionic, butyric, isovaleric, valeric, isocaproic, caproic, 2-methylhexanoic and heptanoic acids) and benzenecarboxylic acids (pyromellitic, trimellitic, hemimellitic, o-phthalic, m-phthalic, p-phthalic, benzoic, salicylic acids and phenol) was carried out using diluted sulfuric acid as the eluent. Silica-based cation-exchange resins (TSKgel SP-2SW and TSKgel CM-2SW) were very suitable for the ion-exclusion chromatographic separation of these benzenecarboxylic acids. Excellent simultaneous separation of these benzenecarboxylic acids was achieved on a TSKgel SP-2SW column (150 x 6 mm I.D.) in 17 min using a 2.5 mM sulfuric acid at pH 2.4 as the eluent. Polymethacrylate-based cation-exchange resins (TSKgel SP-5PW, TSKgel CM-5PW and TSKgel OA-Pak A) acted as advanced stationary phases for the ion-exclusion chromatographic separation of these C1-C7 aliphatic carboxylic acids. Excellent simultaneous separation of these C1-C7 acids was achieved on a TSKgel CM-5PW column (150 x 6 mm I.D.) in 32 min using a 0.05 mM sulfuric acid at pH 4.0 as the eluent.

  7. 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

  8. Hybrid organic-inorganic silica monolith with hydrophobic/strong cation-exchange functional groups as a sorbent for micro-solid phase extraction.

    PubMed

    Zheng, Ming-Ming; Ruan, Ge-Deng; Feng, Yu-Qi

    2009-11-06

    A hybrid organic-inorganic silica monolith with hydrophobic and strong cation-exchange functional groups was prepared and used as a sorbent for micro-solid phase extraction (micro-SPE). The hybrid silica monolith functionalized with octyl and thiol groups was conveniently synthesized by hydrolysis and polycondensation of a mixture of tetraethoxysilane (TEOS), n-octyltriethoxysilane (C8-TEOS) and 3-mercaptopropyltrimethoxysilane (MPTMS) via a two-step catalytic sol-gel process. Due to the favorable chemical reactivity of mercapto pendant moieties, the obtained hybrid monolith was oxidized using hydrogen peroxide (30%, w/w) to yield sulfonic acid groups, which provided strong cation-exchange sites. The obtained hybrid monolith was characterized by diffused infrared spectroscopy, elemental analysis, scanning electron microscopy and mercury intrusion porosimetry. The results show that the resulting monolith contains much higher carbon (31.6%) and sulfur (4.8%) contents than traditionally bonded silica materials. The extraction performance of the hybrid monolith was evaluated using sulfonamides as testing analytes by micro-SPE on-line coupled to HPLC. The results show that the hybrid monolith with hydrophobic and strong cation-exchange functional groups exhibits high extraction efficiency towards the testing analytes. The column-to-column RSD values were 1.3-9.8% for the extraction of SAs investigated. The extraction performance of the hybrid silica monolith remained practically unchanged after treated with acid (pH 1.0) and basic solutions (pH 10.5). Finally, the application of the hybrid monolith was demonstrated by micro-SPE of sulfonamide residues from milk followed by HPLC-UV analysis. The limits of detection (S/N=3) for eight SAs were found to be 1.0-3.0ng/mL in milk. The recoveries of eight SAs spiked in milk sample ranged from 80.2% to 115.6%, with relative standard deviations less than 11.8%.

  9. Simultaneous separation of inorganic anions and cations by using anion-exchange and cation-exchange columns connected in tandem in ion chromatography.

    PubMed

    Karim, Khairil Juhanni Binti Abd; Jin, Ji-Ye; Takeuchi, Toyohide

    2003-05-02

    Inorganic anions and cations in environmental waters were determined by ion chromatography. Stationary and mobile phases were examined for the simultaneous separation of both anions and cations. Cations detection by UV detection requires a mobile phase with a UV absorbing additive, which indirectly visualizes cations as negative peaks. Simultaneous separation of anions and cations were achieved when using an eluent that consists of inorganic acid with weak basic amino acid as additives. It was convenient to separate both anions and cations by coupling anion-exchange and cation-exchange columns in tandem. The order of the separation columns connected affected the elution profiles. When the eluent comprises of multiple anions and a single cation, the anion-exchange column should be connected in the upper stream, whereas when the eluent comprises multiple cations and a single anion, the cation-exchange column should be connected in the upper stream. Use of switching valves also allowed simultaneous separation of anions and cations in a single chromatographic run. In the present work, operating conditions were optimized for the simultaneous separation of anions and cations.

  10. 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.

  11. Ion-exclusion/cation-exchange chromatographic determination of common inorganic ions in human saliva by using an eluent containing zwitterionic surfactant.

    PubMed

    Mori, Masanobu; Iwata, Tomotaka; Satori, Tatsuya; Ohira, Shin-Ichi; Itabashi, Hideyuki; Tanaka, Kazuhiko

    2008-12-12

    Ion-exclusion/cation-exchange chromatography with an eluent containing the bile salt-type zwitterionic surfactant CHAPS was performed in order to evaluate variations in anion (SO(4)(2-), NO(3)(-), and SCN(-)) and cation (Na(+), K(+), NH(4)(+), Mg(2+), and Ca(2+)) concentrations in human saliva. CHAPS prevents the adsorption of proteins to the stationary phase, i.e., weakly acidic cation-exchange resin, since it aggregates proteins without denaturing them. Addition of 1mM CHAPS to the eluent comprising 6mM tartaric acid and 7 mM 18-crown-6 yielded reproducible separations of anions and cations in protein-containing saliva. The resolutions of anions and cations were not significantly affected by the addition of CHAPS to the eluent. The concentrations of Na(+) and K(+) varied before and after meals; or that of SCN(-), upon smoking. The relative standard deviations of peak areas ranged from 0.3 to 5.1% in 1 day (n=20) and from 1.4 to 5.8% over 6 days (n=6).

  12. Selenium speciation in dill (Anethum graveolens L.) by ion pairing reversed phase and cation exchange HPLC with ICP-MS detection.

    PubMed

    Cankur, Oktay; Yathavakilla, Santha K V; Caruso, Joseph A

    2006-11-15

    In the present work, speciation of selenium in dill (Anethum graveolens L.), supplemented with sodium selenite during its growth, was performed using ion pairing reversed phase and cation exchange chromatography. Heptafluorobutyric acid (HFBA) was used as the ion-pairing agent in reversed phase chromatography. In cation exchange chromatography, two different gradient programs were employed for the identification of selenospecies using pyridinium formate as the mobile phase. Low molecular weight selenocompounds were extracted from root, stem and dill leaf with 0.1M HCl. Enzymatic digestion was used for the extraction of selenospecies related to high molecular weight compounds. The chromatograms obtained from different parts of the plant revealed major differences in the type of selenospecies as well as their concentrations. The major selenospecies found in different parts of the plant is Se-methyl-selenocysteine (MeSeCys). Another major Se species identified is Se-methyl-selenomethionine (MeSeMet), which has the highest relative concentration in the root indicating possible Se volatilization from that part of the plant. Selenomethionine (SeMet) is present in minor quantities in all parts of the plant.

  13. A facile cation exchange-based aqueous synthesis of highly stable and biocompatible Ag₂S quantum dots emitting in the second near-infrared biological window.

    PubMed

    Gui, Rijun; Sun, Jie; Liu, Dexiu; Wang, Yanfeng; Jin, Hui

    2014-11-28

    Second near-infrared (NIR-II) emitting Ag2S quantum dots (QDs) with high stability and biocompatibility were synthesized and developed toward an ideal nanoprobe. This study reports a facile synthesis of NIR-II Ag2S QDs on the basis of cation exchange between visible-emitting CdS QDs and Ag(+) ions in aqueous solution. Experimental data testified that the cation exchange was quick and complete and that the resultant products were single monoclinic Ag2S without CdS QDs. The prepared Ag2S QDs were systematically characterized, showed typical NIR-II emission and high PL stability, and had small diameters (~3.5 nm) and a quantum yield up to 2.3%. The results of cytotoxicity assay suggested that the Ag2S QDs produced negligible effects in altering the cell proliferation or in generating reactive oxygen species, indicating an ultralow cytotoxicity and an excellent biocompatibility. These properties have opened up the possibility of using Ag2S QDs for effective bioimaging applications.

  14. 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.

  15. Preparation of a strong-cation exchange monolith by a novel method and its application in the separation of IgG on high performance liquid chromatography.

    PubMed

    Yang, Gengliang; Bai, Ligai; Yan, Cuihong; Gu, Yanzhao; Ma, Junjie

    2011-10-15

    A strong cation-exchange poly(vinyl carboxylate-co-ethyleneglycol dimethacrylate) (poly(VC-co-EDMA)) monolithic column for high performance liquid chromatography (HPLC) has been prepared firstly by atom transfer radical polymerization (ATRP) without the expensive complexing ligand, in which vinyl carboxylate was used as the monomer, ethyleneglycol dimethacrylate as the cross linking agent, carbon tetrachloride as the initiator and ferrous chloride as the catalyst. Conditions of the polymerization have been studied and optimized. Morphology of monolithic materials was studied by scanning electronic microscopy. Chemical groups of the monolith were assayed by infrared spectra method and the pore size distribution was determined by a mercury porosimeter. Moreover, the monolith was modified to bear strong-cation exchange groups and tested on the separation of human immune globulin G (IgG) from human plasma in conjunction with HPLC. Good resolution was obtained in a short time (10 min) in the separation. The effects of pH and buffer concentration on the elution of IgG have been investigated. Moreover, frontal analytical method was used to get the IgG dynamic banding capacity of the monolith that was 3.0 mg g(-1). Besides, the monolith was also used to separate lysozyme from egg white and separate the mixture of papain, snailase and IgG.

  16. 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.

  17. Fast and Efficient Separation and Determination of UV-absorbing Amino Acids, Nucleobases, and Creatinine Using a Carboxy-functionalized Cation-exchange Column.

    PubMed

    Yokoyama, Yukio; Fujishima, Takeru; Kurota, Kazuki

    2015-01-01

    This paper presents a new HPLC technique for the determination of biogenic cations such as amino acids and nucleobases, using a weak-acid cation-exchange column. Fourteen analytes, five amino acids and seven bases in addition to creatinine and creatine, were separated in 12 min by means of a two-liquid gradient elution with UV detection. The newly released column packed with a carboxy-functionalized polymethacrylate resin could give excellent selectivity to the organic cations of interest, although such a column is in general suitable for the separation of inorganic common cations. The chromatographic intra-day repeatability was very good with RSDs less than 0.4%, and the quantitation precision based on peak area intensities was also good with RSDs less than 5% for all analytes. The linear calibration lines for quantitation ranged between 5 and 500 μM on 20-μL injections with R(2) more than 0.9990. Since the method could provide concentration data of urinary creatinine and some metabolites simultaneously, for example, the urinary phenylalanine/creatinine ratios for phenylketonuria of inborn errors of metabolism were simply determined through one chromatographic run. The ratios for patients were significantly higher than those for controls. We found that the new weak-acid cation-exchange column was suitable for the separation of organic cations as well as inorganic cations.

  18. 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.

  19. Magnetic excitations in (SiO 2)Co nano-composite films: Brillouin light scattering study

    NASA Astrophysics Data System (ADS)

    Stashkevich, A. A.; Roussigné, Y.; Stognij, A. I.; Novitskii, N. I.; Wurtz, G.; Zayats, A. V.; Viau, G.; Chaboussant, G.; Ott, F.; Lutsev, L. V.; Djemia, P.; Kostylev, M. P.; Belotelov, V.

    2009-04-01

    Behaviour of magnetic excitations in the Damon-Eshbach (DE) and backward volume (BV) geometries in nano-composite (SiO 2) 100-xCo x (50% at< x<80% at) films has been studied by Brillouin light scattering (BLS). It has been shown that it is the structure of Stokes/anti-Stokes BLS lines in the DE geometry that allows reliable identification of dipole-exchange spin waves (SW) and numerical estimation of the value of the effective exchange constant A eff of a super-ferromagnetic nano-granular sample ( x=80% at).

  20. 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.

  1. 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.

  2. AC impedance analysis of polypyrrole thin films

    NASA Technical Reports Server (NTRS)

    Penner, Reginald M.; Martin, Charles R.

    1987-01-01

    The AC impedance spectra of thin polypyrrole films were obtained at open circuit potentials from -0.4 to 0.4 V vs SCE. Two limiting cases are discussed for which simplified equivalent circuits are applicable. At very positive potentials, the predominantly nonfaradaic AC impedance of polypyrrole is very similar to that observed previously for finite porous metallic films. Modeling of the data with the appropriate equivalent circuit permits effective pore diameter and pore number densities of the oxidized film to be estimated. At potentials from -0.4 to -0.3 V, the polypyrrole film is essentially nonelectronically conductive and diffusion of polymer oxidized sites with their associated counterions can be assumed to be linear from the film/substrate electrode interface. The equivalent circuit for the polypyrrole film at these potentials is that previously described for metal oxide, lithium intercalation thin films. Using this model, counterion diffusion coefficients are determined for both semi-infinite and finite diffusion domains. In addition, the limiting low frequency resistance and capacitance of the polypyrrole thin fims was determined and compared to that obtained previously for thicker films of the polymer. The origin of the observed potential dependence of these low frequency circuit components is discussed.

  3. Formation of Al/B4C Surface Nano-composite Layers on 7075 Al Alloy Employing Friction Stir Processing

    NASA Astrophysics Data System (ADS)

    Kashani-Bozorg, S. F.; Jazayeri, K.

    2009-06-01

    Al/B4C surface nano-composite layers was achieved on commercial 7075 Al substrate employing friction stir processing technique. Agglomeration of B4C particles was occurred after a single pass. The dispersion of B4C particles was found to be affected by the number of FSP passes. A distribution of nano-size B4C particle was achieved after four passes. Moreover, the increasing in number of FSP passes causes a decreasing in matrix grain size of the surface nano-composite layer. The micro hardness of the surface nano-composite layer improves by almost two times as compared to that of the as-received substrate; this is attributed to the finer matrix grains and dispersion of nano-sized B4C particles.

  4. Fabrication of micro-nano composite textured surface for slurry sawn mc-Si wafers cell

    NASA Astrophysics Data System (ADS)

    Niu, Y. C.; liu, Z.; Ren, X. K.; Liu, X. J.; Liu, H. T.; Jiang, Y. S.

    2017-01-01

    In order to enhance the PV efficiency of the cell made from slurry sawn (SS) mc-Si wafers, using a Ag-assisted electroless etching (AgNO3+HF+H2O2) combined with an auxiliary etching (HF+HNO3) the RENA textured SS mc-Si wafers (called as RENA wafers) were further textured (nano pores were formed on the original micro pits) to change into micro-nano composite textured wafers (called as MN-RENA wafers). The solar cells made from the MN-RENA wafers had a better PV efficiency than that of RENA wafers. This is mainly attributed to the higher light-trapping of the micro-nano composite texture. The nano size texture enhanced the light-trap of wafer surface and, at the same time, the micro size texture maintained the light-trap uniformity of different gains of RENA wafer. However, there still exist a potential for optimization, such as, the SiNx passviation coating should be improved to be deposited more uniformly in order to passivate the bottom of pits better and to reduce the reflectance of the obtuse tips of pits.

  5. Controlling the photoluminescence of ZnO:Si nano-composite films by heat-treatment

    SciTech Connect

    Shabnam,; Kant, Chhaya Ravi; Arun, P.

    2010-10-15

    Nano-composite thin films of silicon and zinc oxide were deposited on glass substrates using thermal co-evaporation. On heating the films at different temperatures and different atmospheric pressures, the photoluminescence (PL) emission spectra become broad, giving emissions in UV-Blue, Green and Red region. Analyses reveal that defect-dominated structure of ZnO contributes to the broad PL spectra observed. X-ray diffraction and Raman spectra analysis show that the defects caused by oxygen vacancies decrease with heating which is accompanied by a competing process of decrease in grain size made possible by surrounding silicon reacting at the surface of the ZnO nano-cluster grains giving new bonds, possibly O-Si-Zn bonds. Crystallinity of nano-grains and defects contribute different emission peaks that depending on relative contributions can give comparable peaks resulting in broad emission spectra. The study shows that simple post-deposition process can lead to fabrication of white light emitting devices based on these nano-composites. Best emission spectra are obtained by heating at a temperature of 250 {sup o}C in low vacuum.

  6. Impact of in situ preparation of CdS filled PVP nano-composite.

    PubMed

    Abdelghany, A M; Abdelrazek, E M; Rashad, D S

    2014-09-15

    Cadmium sulfide nanoparticles filled polyvinyl pyrrolidone (PVP) were prepared by in situ wet chemical precipitation technique. X-ray diffraction (XRD), Fourier transforms infrared spectra (FTIR), transmission electron microscopy (TEM) and ultraviolet-visible (UV/Vis) were used to characterize the prepared nano-composites. Density Function Theory (DFT) was used to approve the complexation process. XRD results indicate appearance of two peaks at about 28.1°, 27.4° corresponds to (101) and (002) planes which suggest hexagonal phase of CdS with lattice constants of 4.14, 6.72 Å in the polymeric matrix. UV/Vis spectra reveal that nano-composite films show quantum confinement effect. The absorption showed a shift toward the shorter wavelength (blue shift) with decrease in the concentration of Cd+ ions. Optical band gap and particle size were calculated and is in agreement with the results obtained from TEM data. Transmission electron microscopy shows that the prepared CdS nanoparticles were dispersed and nearly uniform in diameter within the polymeric matrix.

  7. 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.

  8. 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.

  9. Preparation and Characterization of New Nano-Composite Scaffolds Loaded With Vascular Stents

    PubMed Central

    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

  10. Cesium removal from nuclear waste using a magnetical CuHCNPAN nano composite

    NASA Astrophysics Data System (ADS)

    Mobtaker, Hossein Ghasemi; Yousefi, Taher; Pakzad, Seyed Mohammadreza

    2016-12-01

    A nano-composite of copper hexacyanoferrate@polyacrylonitrile@magnetite (CuHCNPAN) was synthesized through chemical co-precipitation. The product were characterized using FT IR, XRD, SEM and TG techniques. The results of FTIR, XRD confirmed the composite formation. The SEM images showed that the particles are 20-60 nm in diameter. The composite showed high mechanical, chemical and thermal stability. The nano composite was used for removal of cesium ions from waste solutions. Effect of various parameters such as contact time, initial concentration, pH, competition ions and temperature were studied. After the metal ion adsorption process the magnetic separation of adsorbent from absorbents was carried out through external magnetic field. Maximum sorption capacity was about 260 mg/g. The kinetic studies showed that the equilibrium was achieved at 5 h and the experimental data fitted by the second order model. The adsorption isotherm was best modeled by Longmuir isotherm. The endothermic and spontaneous (and entropy increasing) nature of sorption process were approved by thermodynamic results. The results cleared which the synthesized CuHCNPAM composite is promising adsorbent for removal of cesium ions from nuclear waste.

  11. Nano-composite insert in 1D waveguides for control of elastic power flow.

    PubMed

    Vignesh, P S; Mitra, Mira; Gopalakrishnan, S

    2007-01-24

    In this paper, carbon nanotube embedded polymer composite/nano-composites are used to regulate power flow from its source to other parts of the structure. This is done by inserting nano-composite strips in the waveguides which are modelled here as isotropic Euler-Bernoulli beams with axial, transverse and rotational degrees of freedom. The power flow is due to wave propagation resulting from a high frequency broadband impulse load. The underlying concept is that the high stiffness of the insert reduces the wave transmission between different parts of the structures. The simulations are done using a wavelet based spectral finite element (WSFE) technique which is specially tailored for such high frequency wave propagation analysis. Numerical experiments are performed to illustrate the use of inserts in maintaining the power flow in a certain region of the structure below a given threshold value which may be specified depending on various applications. The effects of parameters such as the volume fraction of carbon nanotube (CNT) in the polymer, and the length and position of the inserts are also studied. These studies help in defining the optimal volume fraction of CNT and length of the insert for a specified structural configuration.

  12. 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.

  13. 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.

  14. Lithium-doped hydroxyapatite nano-composites: Synthesis, characterization, gamma attenuation coefficient and dielectric properties

    NASA Astrophysics Data System (ADS)

    Badran, H.; Yahia, I. S.; Hamdy, Mohamed S.; Awwad, N. S.

    2017-01-01

    Lithium-hydroxyapatite (0, 1, 5, 10, 20, 30 and 40 wt% Li-HAp) nano-composites were synthesized by sol-gel technique followed by microwave-hydrothermal treatment. The composites were characterized by X-ray diffraction (XRD), Field emission scanning electron microscope (FE-SEM), energy dispersive spectroscopy (EDS), Fourier transform infrared (FTIR) and Raman techniques. Gamma attenuation coefficient and the dielectric properties for all composites were investigated. The crystallinity degree of Li-doped HAp was higher than that of un-doped HAp. Gamma attenuation coefficient values increased from 0.562 cm-1 for 0 wt% Li-HAp to 2.190 cm-1 for 40 wt% Li-HAp. The alternating current conductivity increased with increasing frequency. The concentration of Li affect the values of dielectric constant where Li doped HAp of low dielectric constant can have an advantage for healing in bone fractures. The calcium to phosphorus ratio decreased from 1.43 to 1.37 with the addition of lithium indicating the Ca deficiency in the studied composites. Our findings lead to the conclusion that Li-HAp is a new nano-composite useful for medical applications and could be doped with gamma shield materials.

  15. Preparation and Electrical Property of Polypyrrole-Polyethylene Composite

    NASA Astrophysics Data System (ADS)

    Yoshino, Katsumi; Yin, Xiao Hong; Morita, Shigenori; Nakanishi, Yutaka; Nakagawa, Shinichi; Yamamoto, Hideo; Watanuki, Toshiro; Isa, Isao

    1993-02-01

    Polypyrrole-polyethylene composites have been prepared by pressing the mixture of polypyrrole coated and non-coated polyethylene spheres. Electrical conductivity is enhanced by more than 16 orders of magnitude and its activation energy decreases remarkably at concentration of polypyrrole coated polyethylene above around 10-20%, which corresponds to effective polypyrrole concentration of 0.1-0.2%. These characteristics can be explained by a percolation model. That is, at this concentration electrodes are bridged by conducting channel of doped polypyrrole. Thermoelectric power increases in proportion to absolute temperature and is independent on concentration of polypyrrole coated polyethylene sphere above 30%, which support the percolation model. The electrical property of this polypyrrole-polyethylene composite is found to be stable up to 160°C. The application of this composite to the semiconducting layer of a cable has been proposed.

  16. Surface plasmon resonance and magneto-optical enhancement on Au-Co nano-composite thin films

    SciTech Connect

    Yang, K.; Clavero, C.; Skuza, J. R.; Varela del Arco, Maria; Lukaszew, R. A.

    2007-01-01

    We present our investigations on the enhancement of magneto-optical effects in nano-composite Au-Co thin films. All the samples in this study were obtained by co-sputter deposition varying the relative Au:Co composition and the growth temperature. A strong enhancement of the transverse magneto-optical activity is observed when surface plasmons are excited in the Krestchmann configuration. The correlation between the nano-composite films microstructure, morphology, composition, and their optical response under surface plasmon resonance excitation and their magneto-optical enhancement leading to enhanced sensing capability is discussed.

  17. Polypyrrole actuators for tremor suppression

    NASA Astrophysics Data System (ADS)

    Skaarup, Steen; Mogensen, Naja; Bay, Lasse; West, Keld

    2003-07-01

    Neurological tremor affecting limbs can be divided into at least 6 different types with frequencies ranging from 2 to about 20 Hz. In order to alleviate the symptoms by suppressing the tremor, sensing and actuation systems able to perform at these frequencies are needed. Electroactive polymers exemplify "soft actuator" technology that may be especially suitable for use in conjunction with human limbs. The electrochemical and mechanical properties of polypyrrole dodecyl benzene sulphonate actuator films have been studied with this application in mind. The results show that the time constants for the change of length and for the stiffness change are significantly different; the stiffness change being about 10 times faster. Both force measurements and Electrochemical Quartz Crystal Microbalance measurements indicate that the actuation process is complex and involves at least two different processes. The EQCM results make it possible to formulate a hypothesis for the two different time constants: Sodium ions enter the polymer correlated with a fast mass change that probably involves a few (~4) strongly bound water molecules as well. On further reduction, about 10 additional water molecules enter the polymer in a slower process driven by osmotic pressure. Earlier work has tended to focus on achieving the maximum length change, therefore taking the time needed to include all processes. However, since the slower process described above is associated with the lowest strength of the actuator, concentrating on the faster stiffness change results in only a small reduction in the work done by the actuator. This may make actuation at higher frequencies feasible.

  18. 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

    2016-07-05

    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.

  19. 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

  20. 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

  1. The effect of chelating agent on the separation of Fe(III) and Ti(IV) from binary mixture solution by cation-exchange membrane.

    PubMed

    Kir, Esengül; Cengeloğlu, Yunus; Ersöz, Mustafa

    2005-12-15

    The competitive transport of Fe(III) and Ti(IV) ions and the effect of chelating agents on separation from binary mixture solutions through charged polysulfone cation-exchange membrane (SA3S) has been studied under Donnan dialysis conditions. The amount of chelating agent was taken as an equimolar of Fe(III) ion in the feed phase. In this process, the membrane separated two electrolyte solutions: the feed solution, initially containing metal salts (Fe, Ti), or metal salts solution, containing a chelating agent, and the other side (receiver solution) being HCl solution. An external potential field is not applied. It was observed that the chelating agents affect the metal transport; the transport of Fe(III) is decreased and the transport of Ti(IV) is increased.

  2. 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.

  3. 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.

  4. Automated liquid chromatographic determination of atenolol in plasma using dialysis and trace enrichment on a cation-exchange precolumn for sample handling.

    PubMed

    Chiap, P; Buraglia, B M; Ceccato, A; Hubert, P; Crommen, J

    2000-02-28

    A fully automated method involving dialysis combined with trace enrichment was developed for the liquid chromatographic (LC) determination of atenolol, a hydrophilic beta-blocking agent, in human plasma. The plasma samples were dialysed on a cellulose acetate membrane and the dialysate was reconcentrated on a short trace enrichment column (TEC) packed with a strong cation-exchange material. All sample handling operations can be executed automatically by a sample processor (ASTED system). After TEC conditioning, the plasma sample, to which the internal standard (sotalol, another hydrophilic beta-blocker) was automatically added, was introduced in the donor channel and dialysed in the static/pulsed mode. The dialysis liquid consisted of 4.3 mM phosphoric acid. When the dialysis process was discontinued, the analytes were eluted from the TEC in the back-flush mode by the LC mobile phase and transferred to the analytical column, packed with octyl silica. The LC mobile phase consisted of phosphate buffer, pH 7.0-methanol (81:19; v/v) with 1-octanesulfonate. Atenolol and the internal standard were monitored photometrically at 225 nm. The different parameters influencing the dialysis and trace enrichment processes were optimised with respect to analyte recovery. The influence of two different kinds of cation-exchange material on analyte recovery and peak efficiency was also studied. The method was then validated in the concentration range 25-1000 ng/ml. The mean recovery for atenolol was 65% and the limit of quantitation was 25 ng/ml.

  5. 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

    2016-01-05

    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.

  6. Carbon nanotube-reinforced carbon nano-composite fibrils by electro-spinning

    NASA Astrophysics Data System (ADS)

    Ali, Ashraf Abd El-Fattah

    Fibers of Polyacrylonitrile (PAN) are the precursor of 90% of produced carbon fibers. It is generally thought that the better the degree of molecular orientation in the original PAN fiber, the better the mechanical properties, in particular the modulus of the resultant fibers. Electro-spinning is a unique process in that it is able to produce polymer fibers having diameters ranging over several orders of magnitude, from the micrometer range typical of conventional fibers down to the nanometer range. Until now and based on the literature review the shape and pattern of produced fibers in all electro-spun polymer solutions have taken an in-plan random pattern and affected by the shape of the collector, which gives a limitation of using these ultra fine produced fibers in textile applications. A notable phenomenon has been recognized under certain spinning conditions for PAN solution, which enable the production of continuous yarn containing partially oriented nano-fibers. This phenomenon opened the door to achieve many objectives such as the production of carbon-carbon nano composites by dispersing (CNT) of superior physical properties inside the PAN polymer solution and producing continues carbon nanotube reinforced PAN based carbon nano composite fibrils. The present study is an attempt to optimize the electro-spinning process for nano-scale fibers, understand the electro-mechanics of electro-spun continuous nano-fiber yarns, stabilize, carbonize and graphitize of nano fiber yarns with and without CNT and finally study the physical, chemical and mechanical properties of the produced carbon nanotube reinforced PAN based carbon nano composite fibrils before and after heat treatments. The HREM results showed a good alignment for the CNT inside the PAN based carbon nano fiber composites as well as an increase in the crystallite size up to 5nm, which calculated based on Raman spectroscopy measurements. The AFM showed a two-folds increase in the composite modulus more

  7. Improvement of mechanical and thermal properties of high energy electron beam irradiated HDPE/hydroxyapatite nano-composite

    NASA Astrophysics Data System (ADS)

    Mohammadi, M.; Ziaie, F.; Majdabadi, A.; Akhavan, A.; Shafaei, M.

    2017-01-01

    In this research work, the nano-composites of high density polyethylene/hydroxyapatite samples were manufactured via two methods: In the first method, the granules of high density polyethylene and nano-structure hydroxyapatite were processed in an internal mixer to prepare the nano-composite samples with a different weight percentage of the reinforcement phase. As for the second one, high density polyethylene was prepared in nano-powder form in boiling xylene. During this procedure, the hydroxyapatite nano-powder was added with different weight percentages to the solvent to obtain the nano-composite. In both of the procedures, the used hydroxyapatite nano-powder was synthesized via hydrolysis methods. The samples were irradiated under 10 MeV electron beam in 70-200 kGy of doses. Mechanical, thermal and morphological properties of the samples were investigated and compared. The results demonstrate that the nano-composites which we have prepared using nano-polyethylene, show better mechanical and thermal properties than the composites prepared from normal polyethylene granules, due to the better dispersion of nano-particles in the polymer matrix.

  8. BaM/YIG nano-composites: A microwave material for C to U band application

    NASA Astrophysics Data System (ADS)

    Sharma, Vipul; Kumari, Sweta; Kuanr, Bijoy Kumar

    2017-05-01

    Hexaferrites have become important candidates for a variety of microwave and millimeter wave devices due to their large uniaxial magneto-crystalline anisotropy and high saturation magnetization. The goal of the present investigation is to synthesize Barium hexaferrite/Yttrium Iron Garnet (BaFe12O19/Y3Fe5O12): (BaM/YIG) Nano-Composites (NCs) to be used in broad band microwave frequency range applications, especially as microwave absorber. X-ray diffractometry, Vibrating Sample Magnetometer (VSM), and ferromagnetic resonance (FMR) techniques were used to characterize these NCs. Using a Cu coplanar wave guide and a Vector Network Analyzer, broadband (C to U) microwave absorption were investigated by placing the bulk sample in flip chip mode. Various mathematical models were employed to fit the experimental data to yield intrinsic and extrinsic damping parameters.

  9. Macroscopic Ordering of CNTs in a Liquid Crystalline Polymer Nano-Composite by Shearing

    NASA Astrophysics Data System (ADS)

    Kalakonda, P.; Sarkar, S.; Iannacchione, G. S.; Gombos, E.; Hoonjan, G. S.; Georgiev, G.; Cebe, P.

    2012-02-01

    We present a series of complimentary experiments exploring the macroscopic alignment of carbon nanotubes (CNTs) in a liquid crystalline polymer (isotactic polypropylene - iPP) nano-composites as a function of temperature, shear, and CNT concentration. The phase behavior of iPP+CNT, studied by Modulated Differential Scanning Calorimetry, revealed the evolution of the α-monoclinic transition and its dynamics, which are dependent on CNT content and thermal treatment. These results indicate that the CNT nucleates crystal formation from the melt. Spectroscopic ellipsometry reveals a change in the optical constants that are connected to the ordering of CNTs when the iPP+CNT is sheared. This anisotropy is also exhibited in measurements of the electrical and thermal conductivities parallel and perpendicular to the shear direction. The amount of order induced into the dispersed CNTs is relatively low for these low concentration samples (< 5 wt%).

  10. 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.

  11. 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

  12. 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.

  13. Nano-composite Si particle formation by plasma spraying for negative electrode of Li ion batteries

    NASA Astrophysics Data System (ADS)

    Kambara, M.; Kitayama, A.; Homma, K.; Hideshima, T.; Kaga, M.; Sheem, K.-Y.; Ishida, S.; Yoshida, T.

    2014-04-01

    Nano-composite silicon powders have been produced at a maximum process throughput of 6 g/min by plasma spraying with metallurgical grade silicon powder as raw material. The obtained powders are found to be fundamentally composed of crystalline silicon particles of 20-40 nm in diameter, and are coated with an ˜5-nm-thick amorphous carbonous layer when methane gas is additionally introduced during plasma spraying. The performance of half-cell batteries containing the powders as negative electrodes has shown that the capacity decay observed for the raw Si coarse particles is significantly improved by plasma treatment. The carbonous coating potentially contributes to an improvement in capacity retention, although coexisting SiC particles that inevitably form during high-temperature processing reduce the overall capacity.

  14. Nitrate removal by Fe0/Pd/Cu nano-composite in groundwater.

    PubMed

    Liu, Hongyuan; Guo, Min; Zhang, Yan

    2014-01-01

    Nitrate pollution in groundwater shows a great threat to the safety of drinking water. Chemical reduction by zero-valent iron is being considered as a promising technique for nitrate removal from contaminated groundwater. In this paper, Fe0/Pd/Cu nano-composites were prepared by the liquid-phase reduction method, and batch experiments of nitrate reduction by the prepared Fe0/Pd/Cu nano-composites under various operating conditions were carried out. It has been found that nano-Fe0/Pd/Cu composites processed dual functions: catalytic reduction and chemical reduction. The introduction of Pd and Cu not only improved nitrate removal rate, but also reduced the generation of ammonia. Nitrate removal rate was affected by the amount of Fe0/Pd/Cu, initial nitrate concentration, solution pH, dissolved oxygen (DO), reaction temperature, the presence of anions, and organic pollutant. Moreover, nitrate reduction by Fe0/Pd/Cu composites followed the pseudo-first-order reaction kinetics. The removal rate of nitrate and total nitrogen were about 85% and 40.8%, respectively, under the reaction condition of Fe-6.0%Pd-3.0%Cu amount of 0.25 g/L, pH value of 7.1, DO of 0.42 mg/L, and initial nitrate concentration of 100 mg/L. Compared with the previous studies with Fe0 alone or Fe-Cu, nano-Fe-6%Pd-3%Cu composites showed a better selectivity to N2.

  15. 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.

  16. Cooperative cytotoxic activity of Zn and Cu in bovine serum albumin-conjugated ZnS/CuS nano-composites in PC12 cancer cells

    NASA Astrophysics Data System (ADS)

    Wang, Hua-Jie; Yu, Xue-Hong; Wang, Cai-Feng; Cao, Ying

    2013-11-01

    Series of self-assembled and mono-dispersed bovine serum albumin (BSA)-conjugated ZnS/CuS nano-composites with different Zn/Cu ratios had been successfully synthesized by a combination method of the biomimetic synthesis and ion-exchange strategy under the gentle conditions. High-resolution transmission electron microscopy observation, Fourier transform infrared spectra and zeta potential analysis demonstrated that BSA-conjugated ZnS/CuS nano-composites with well dispersity had the hierarchical structure and BSA was a key factor to control the morphology and surface electro-negativity of final products. The real-time monitoring by atomic absorption spectroscopy and powder X-ray diffraction revealed that the Zn/Cu ratio of nano-composites could be controlled by adjusting the ion-exchange time. In addition, the metabolic and morphological assays indicated that the metabolic proliferation and spread of rat pheochromocytoma (PC12) cells could be inhibited by nano-composites, with the high anti-cancer activity at a low concentration (4 ppm). What were more important, Zn and Cu in nano-composites exhibited a positive cooperativity at inhibiting cancer cell functions. The microscope observation and biochemical marker analysis clearly revealed that the nano-composites-included lipid peroxidation and disintegration of membrane led to the death of PC12 cells. Summarily, the present study substantiated the potential of BSA-conjugated ZnS/CuS nano-composites as anti-cancer drug.

  17. 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.

  18. Role of competitive cation exchange on chromatographic displacement of cesium in the vadose zone beneath the Hanford S/SX tank farm

    SciTech Connect

    Lichtner, Peter C.; Yabusaki, Steve; Pruess, Karsten; Steefel, Carl I.

    2003-10-01

    Migration of radionuclides under the SX-tank farm at the Hanford nuclear waste complex involves interaction of variably water saturated sediments with concentrated NaOH-NaNO3-NaNO2 solutions that have leaked from the tanks. Constant Kd models for describing radionuclide retardation are not valid under these conditions because of strong competition for sorption sites by abundant Na+ ions, and because of dramatically changing solution compositions with time as the highly concentrated tank fluid becomes diluted as it mixes with infiltrating rainwater. A mechanistic multicomponent sorption model is required that can account for effects of competition and spatially and temporally variable solution compositions. To investigate the influence of the high ionic strength tank fluids on Cs+ migration, numerical calculations are performed using the multiphase-multicomponent reactive transport code FLOTRAN. The computer model describes reactive transport in nonisothermal, variably saturated porous media including both liquid and gas phases. Pitzer activity coefficient corrections are used to describe the high ionic strength solutions. The calculations take into account multicomponent cation exchange based on measured selectivity coefficients specific to the Hanford sediments. Solution composition data obtained from Well 299-W23-19, documenting a moderately concentrated leak from the SX-115 tank, are used to calibrate the model. In addition to exchange of cations Na+, K+, Ca2+, and Cs+, aqueous complexing and a kinetic description of precipitation and dissolution of calcite are also included in the calculations. The fitted infiltration rate of 0.08 m yr-1, and fitted cation exchange capacity of 0.05 mol kg-1 are consistent with measured values for the Hanford sediments. A sensitivity analysis is performed for Na+ concentrations ranging from 5 to 20 m to investigate the mobility of Cs+ interacting with a highly concentrated background electrolyte solution believed to have been

  19. Lanthanide N,N'-piperazine-bis(methylenephosphonates) (Ln=La, Ce, Nd) that display flexible frameworks, reversible hydration and cation exchange

    SciTech Connect

    Mowat, John P.S.; Groves, John A.; Wharmby, Michael T.; Miller, Stuart R.; Li Yang; Lightfoot, Philip; Wright, Paul A.

    2009-10-15

    Hydrothermal syntheses of lanthanide bisphosphonate metal organic frameworks comprising the light lanthanides lanthanum, cerium and neodymium and N,N'-piperazine bis(methylenephosphonic acid) (H{sub 2}L(1) and its 2-methyl and 2,5-dimethyl derivatives (H{sub 2}L(2) and H{sub 2}L(3)) gives three new structure types. At elevated starting pH (ca. 5 and above) syntheses give 'type I' materials with all metals and acids of the study (MLnLxH{sub 2}O, M=Na, K, Cs; Ln=La, Ce, Nd; x{approx}4: KCeL(1).4H{sub 2}O, C2/c, a=23.5864(2) A, b=12.1186(2) A, c=5.6613(2) A, beta=93.040(2){sup o}). The framework of structure type I shows considerable flexibility as the ligand is changed, due mainly to rotation around the -N-CH{sub 2}- bond of the linker in response to steric considerations. Type I materials demonstrate cation exchange and dehydration and rehydration behaviour. Upon dehydration of KCeL.4H{sub 2}O, the space group changes to P2{sub 1}/n, a=21.8361(12) A, b=9.3519(4) A, c=5.5629(3) A, beta=96.560(4){sup o}, as a result of a change of the piperazine ring from chair to boat configuration. When syntheses are performed at lower pH, two other structure types crystallise. With the 'non-methyl' ligand 1, type II materials result (LnL(1)H{sub 2}L(1).4.5H{sub 2}O: Ln=La, P-1, a=5.7630(13) A, b=10.213(2) A, c=11.649(2) A, alpha=84.242(2){sup o}, beta=89.051(2){sup o}, gamma=82.876(2){sup o}) in which one half of the ligands coordinate via the piperazine nitrogen atoms. With the 2-methyl ligand, structure type III crystallises (LnHL(2).4H{sub 2}O: Ln=Nd, Ce, P2{sub 1}/c, a=5.7540(9) A, b=14.1259(18) A, c=21.156(5) A, beta=90.14(2){sup o}) due to unfavourable steric interactions of the methyl group in structure type II. - Graphical abstract: The lanthanides La, Ce and Nd give a family of metal organic frameworks based on N,N'-piperazinebismethylenephosphonate ligands: these display reversible dehydration, structural flexibility and cation exchange.

  20. 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).

  1. 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

  2. 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.

  3. Electrogenerated chemiluminescence detector based on Ru(bpy)32+ immobilized in cation exchange resin for high-performance liquid chromatography: An approach to stable detection

    NASA Astrophysics Data System (ADS)

    Sun, Yonghua; Zhang, Zhujun; Zhang, Xinfeng

    2013-12-01

    In this work, an electrogenerated chemiluminescence (ECL) detector with improved stability was developed for high-performance liquid chromatography (HPLC) detection of hydrochlorothiazide (HCTZ). The detector was prepared by packing cation exchanged resin particles in a glass tube, followed by inserting Pt wires (working electrode) in this tube and sealing. The leakage of Ru(bpy)32+ from the resin was compensated by adding a small amount of Ru(bpy)32+ in the mobile phase. Factors affected the performance of the proposed ECL detector were investigated. Under the optimal conditions, the ECL intensity has a linear relationship with the concentration of HCTZ in the range of 5.0 × 10-8 g mL-1 - 2.5 × 10-5 g mL-1 and the detection limit was 2.0 × 10-8 g mL-1 (S/N = 3). Application of the detector to the analysis of HCTZ in human serum proved feasible.

  4. Cation-exchange high-performance liquid chromatography for variant hemoglobins and HbF/A2: What must hematopathologists know about methodology?

    PubMed Central

    Sharma, Prashant; Das, Reena

    2016-01-01

    Cation-exchange high-performance liquid chromatography (CE-HPLC) is a widely used laboratory test to detect variant hemoglobins as well as quantify hemoglobins F and A2 for the diagnosis of thalassemia syndromes. It’s versatility, speed, reproducibility and convenience have made CE-HPLC the method of choice to initially screen for hemoglobin disorders. Despite its popularity, several methodological aspects of the technology remain obscure to pathologists and this may have consequences in specific situations. This paper discusses the basic principles of the technique, the initial quality control steps and the interpretation of various controls and variables that are available on the instrument output. Subsequent sections are devoted to methodological considerations that arise during reporting of cases. For instance, common problems of misidentified peaks, totals crossing 100%, causes of total area being above or below acceptable limits and the importance of pre-integration region peaks are dealt with. Ultimately, CE-HPLC remains an investigation, the reporting of which combines in-depth knowledge of the biological basics with more than a working knowledge of the technological aspects of the technique. PMID:27019794

  5. Iminodiacetic acid functionalized cation exchange resin for adsorptive removal of Cr(VI), Cd(II), Ni(II) and Pb(II) from their aqueous solutions.

    PubMed

    Misra, R K; Jain, S K; Khatri, P K

    2011-01-30

    Iminodiacetic acid functionality has been introduced on styrene-divinyl benzene co-polymeric beads and characterized by FT-IR in order to develop weak acid based cation exchange resin. This resin was evaluated for the removal of different heavy metal ions namely Cd(II), Cr(VI), Ni(II) and Pb(II) from their aqueous solutions. The results showed greater affinity of resin towards Cr(VI) for which 99.7% removal achieved in optimal conditions following the order Ni(II)>Pb(II)>Cd(II) with 65%, 59% and 28% removal. Experiments were also directed towards kinetic studies of adsorption and found to follow first order reversible kinetic model with the overall rate constants 0.3250, 0.2393, 0.4290 and 0.2968 for Cr(VI), Ni(II), Pb(II) and Cd(II) removal respectively. Detailed studies of Cr(VI) removal has been carried out to see the effect of pH, resin dose and metal ion concentration on adsorption and concluded that complexation enhanced the chromium removal efficacy of resin drastically, which is strongly pH dependent. The findings were also supported by the comparison of FT-IR spectra of neat resin with the chromium-adsorbed resin.

  6. Analysis of amphetamine and methamphetamine in municipal wastewater influent and effluent using weak cation-exchange SPE and LC-MS/MS.

    PubMed

    Boles, Tammy H; Wells, Martha J M

    2016-12-01

    Amphetamine and methamphetamine are emerging contaminants-those for which no regulations currently require monitoring or public reporting of their presence in our water supply. In this research, a protocol for weak cation-exchange (WCX) SPE coupled with LC-MS/MS was developed for determination of emerging contaminants amphetamine and methamphetamine in a complex wastewater matrix. Gradient LC parameters were adjusted to yield baseline separation of methamphetamine from other contaminants. Methamphetamine-D5 was used as the internal standard (IS) to compensate for sample loss during SPE and for signal loss during MS (matrix effects). Recoveries were 102.1 ± 7.9% and 99.4 ± 4.0% for amphetamine and methamphetamine, respectively, using WCX sorbent. Notably, methamphetamine was determined to be present in wastewater influent at each sampling date tested. Amphetamine was present in wastewater influent on two of four sampling dates. Amphetamine concentrations ranged from undetectable to 86.4 ng/L in influent, but it was undetectable in wastewater effluent. Methamphetamine was detected in influent at concentrations ranging from 27.0-60.3 ng/L. Methamphetamine concentration was reduced but incompletely removed at this facility. Although absent in one post-UV effluent sample, concentrations of methamphetamine ranged from 10.8-14.8 ng/L.

  7. Quantitative determination of corticosteroids in bovine milk using mixed-mode polymeric strong cation exchange solid-phase extraction and liquid chromatography-tandem mass spectrometry.

    PubMed

    Tölgyesi, Adám; Tölgyesi, László; Sharma, Virender K; Sohn, Mary; Fekete, Jeno

    2010-12-01

    A new method was developed to identify and quantify corticosteroids (prednisolone, methylprednisone, flumetasone, dexamethasone, and methylprednisolone) in raw bovine milk by liquid chromatography-tandem mass spectrometry (LC-MS/MS) utilizing mixed-mode polymeric strong cation exchange and reversed-phase (MCX) solid-phase extraction (SPE) to reduce ion effects in a multimode ion (MMI) source. The main advantage of this method over other commonly used methods includes the use of a single SPE cartridge with a low volume for sample preparation and fast separation on the HPLC system with reduced ion suppression. This study is the first to report the determination of methylprednisone, a metabolite of methylprednisolone, in bovine milk. This method was validated in accordance with the European Union (EU) Commission Decision 2002/657/EC. The recoveries vary between 90% and 105%. The within-laboratory reproducibility (precision) is less than 30%. The decision limits and detection capabilities were calculated along with LODs, which ranged from 0.02 to 0.07 microg/kg. The method was further enhanced by its successful adaptation to other LC-MS/MS systems equipped with the newly developed ion source, Agilent Jet Stream (AJS). After optimization of the AJS ion source and MS parameters, even lower LOD values were achieved (0.001-0.006 microg/kg) for the corticosteroids. Analytical results obtained with the AJS were characterized by an enhanced area response and similar noise level comparable to those obtained with conventional orthogonal atmospheric ionization (API).

  8. Electrogenerated chemiluminescence detector based on Ru(bpy)3(2+) immobilized in cation exchange resin for high-performance liquid chromatography: An approach to stable detection.

    PubMed

    Sun, Yonghua; Zhang, Zhujun; Zhang, Xinfeng

    2013-12-01

    In this work, an electrogenerated chemiluminescence (ECL) detector with improved stability was developed for high-performance liquid chromatography (HPLC) detection of hydrochlorothiazide (HCTZ). The detector was prepared by packing cation exchanged resin particles in a glass tube, followed by inserting Pt wires (working electrode) in this tube and sealing. The leakage of Ru(bpy)3(2+) from the resin was compensated by adding a small amount of Ru(bpy)3(2+) in the mobile phase. Factors affected the performance of the proposed ECL detector were investigated. Under the optimal conditions, the ECL intensity has a linear relationship with the concentration of HCTZ in the range of 5.0 × 10(-8) g mL(-1)-2.5 × 10(-5) g mL(-1) and the detection limit was 2.0 × 10(-8) g mL(-1) (S/N=3). Application of the detector to the analysis of HCTZ in human serum proved feasible.

  9. 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.

  10. Measurement of cation exchange capacity (CEC) of plant cell walls by X-ray microanalysis (EDX) in the transmission electron microscope.

    PubMed

    Fritz, Eberhard

    2007-08-01

    Cation exchange capacity (CEC) characterizes the number of fixed negative charges of plant cell walls and is an important parameter in studies dealing with the uptake of ions into plant tissues, especially in roots. Conventional methods of CEC determination use bulk tissue, the results are the mean of many cells, and differences in the CEC of different tissue types are masked. Energy-dispersive microanalysis (EDX) in the transmission electron microscope allows CEC determinations on much finer scales. Shoot and fine root tissue of Picea abies was acid washed to remove exchangeable cations. Tissue blocks or semithin tissue sections were loaded with 0.2 mM CaCl2, AlCl3, or Pb(NO3)2 at pH 4.0. The amount of Ca, Al, or Pb adsorbed to the exchange sites of cell walls was determined by EDX. The CEC of cell walls of different tissue types was highly different, ranging in shoot tissues from 0 to 856 mM Ca and 5.8 to 1463 mM Al (block loading) or 4.3 to 1116 mM Ca and 0 to 2830 mM Al (section loading). In root tissue, Pb adsorption to semithin sections yielded CEC values between 29.1 and 954 mM Pb. In most P. abies shoot tissues, the binding capacity was clearly higher for Al than for Ca.

  11. 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.

  12. Noble-Metal-Free Janus-like Structures by Cation Exchange for Z-Scheme Photocatalytic Water Splitting under Broadband Light Irradiation.

    PubMed

    Yuan, Qichen; Liu, Dong; Zhang, Ning; Ye, Wei; Ju, Huanxin; Shi, Lei; Long, Ran; Zhu, Junfa; Xiong, Yujie

    2017-03-15

    Z-scheme water splitting is a promising approach based on high-performance photocatalysis by harvesting broadband solar energy. Its efficiency depends on the well-defined interfaces between two semiconductors for the charge kinetics and their exposed surfaces for chemical reactions. Herein, we report a facile cation-exchange approach to obtain compounds with both properties without the need for noble metals by forming Janus-like structures consisting of γ-MnS and Cu7 S4 with high-quality interfaces. The Janus-like γ-MnS/Cu7 S4 structures displayed dramatically enhanced photocatalytic hydrogen production rates of up to 718 μmol g(-1)  h(-1) under full-spectrum irradiation. Upon further integration with an MnOx oxygen-evolution cocatalyst, overall water splitting was accomplished with the Janus structures. This work provides insight into the surface and interface design of hybrid photocatalysts, and offers a noble-metal-free approach to broadband photocatalytic hydrogen production.

  13. 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

  14. [Rapid analysis of melamine in milk and milk powder using QuEChERS approach coupled with weak cation exchange chromatography].

    PubMed

    Wei, Jie; Guo, Zhimou; Shen, Aijin; Zhang, Feifang; Liang, Xinmiao

    2011-07-01

    A simple, rapid method for the determination of melamine in milk and milk powder was developed using QuEChERS approach coupled with weak cation exchange chromatography (WCX). The samples were extracted and cleaned-up by medicinal alcohol and lipid adsorbent (LAS) simultaneously, then centrifuged and filtered for high performance liquid chromatographic (HPLC) analysis. The separation was performed on a WCX column (150 mm x 4.6 mm, 5 microm) with 2 mmol/L KH2 PO4 (pH 3.8) as mobile phase. The flow rate was 1.5 mL/min and the detection wavelength was 208 nm. The injection volume was 20 microL and the column temperature was 30 degrees C. Under the optimized conditions, good linearity was obtained in the range of 0.02-20 mg/L with a correlation coefficient (r2) of 0.999 9. For samples spiked with melamine standard in the range of 1-50 mg/kg, the average recoveries of standard in the milk and milk powder were 98.9%-105.2% and 86.4%-102.9%, respectively. The relative standard deviations were 0.9%-3.4% and 1.5%-6.7%, respectively. The limits of detection (LOD, S/N > or = 3) were 0.05 mg/kg (milk) and 0.1 mg/kg (milk powder). The present method is green due to not use of the toxic organic solvents.

  15. Analysis of amphetamine-type stimulants and their metabolites in plasma, urine and bile by liquid chromatography with a strong cation-exchange column-tandem mass spectrometry.

    PubMed

    Kuwayama, Kenji; Inoue, Hiroyuki; Kanamori, Tatsuyuki; Tsujikawa, Kenji; Miyaguchi, Hajime; Iwata, Yuko T; Miyauchi, Seiji; Kamo, Naoki

    2008-05-01

    The aim of this work was to develop and validate a method for analysing amphetamine-type stimulants (ATSs) and their metabolites in plasma, urine and bile by liquid chromatography with a strong cation-exchange column-tandem mass spectrometry, and to apply it to the pharmacokinetic study of ATSs. 3,4-Methylenedioxymethamphetamine, methamphetamine, ketamine and their main metabolites, 4-hydroxy-3-methoxymethamphetamine, 3,4-methylenedioxyamphetamine, p-hydroxymethamphetamine, amphetamine and norketamine, were simultaneously quantified by the new method (50-5000 ng/ml). The coefficients of variation and the percent deviations for the eight compounds were in the range of 0.2 to 5.3% and -9.4 to +12.8%, respectively. The recoveries were over 90% in all biological samples tested. This method was effective for the separation and the identification of ATSs and their main metabolites having amine moieties in plasma, urine and bile, and was applicable to pharmacokinetic analysis of methamphetamine, ketamine and their main metabolites in biological samples. This analytical method should be useful for the pharmacokinetic analysis of ATSs.

  16. 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.

  17. 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.

  18. [Preparation of strong cation exchange packings based on monodisperse hydrophilic non-porous resins and their application for fast separation of proteins].

    PubMed

    Zhu, Jinxia; Bo, Chunmiao; Gong, Bolin

    2006-03-01

    Monodisperse, 3.0 microm non-porous hydrophilic poly (glycidylmethacrylate-co-ethylenedimethacrylate) particles were prepared by an one-step swelling and polymerization method. The particles were modified to be a strong cation exchange (SCX) stationary phase for high performance liquid chromatography (HPLC) in the following steps. First, the particles were completely hydrolyzed. Second, the hydrolyzed particles were treated with epichlorhydrin followed by another hydrolysis of the newly introduced epoxide groups. Third, the particles were reacted with chlorosulfonic acid. The SCX stationary phase was evaluated in light of the ion exchange property, separability and hydrophilicity on the separation and retention of proteins in detail. Four proteins were quickly separated in 1.0 min with linear gradient elution using the synthesized SCX stationary phase. It was found that it followed ion exchange chromatographic (IEC) retention mechanism. The SCX resin was used for the fast purification of lysozyme from egg white and cytochrome-C from pig heart in 3.0 min with only one step. The results obtained were satisfactory.

  19. [Preparation of weak cation-exchange packings based on monodisperse porous poly (chloromethylstyrene-co-divinylbenzene) beads and its applications in separation of biopolymers].

    PubMed

    Li, Long; Ma, Guijuan; Gong, Bolin

    2005-11-01

    Monodisperse polystyrene seed particles were prepared by dispersion polymerization of styrene in ethanol and water under a nitrogen atmosphere using benzoyl peroxide as an initiator. Then the monodisperse, porous poly (chloromethylstyrene-co-divinylbenzene) beads in the range of 6 - 15 microm were prepared by one-step swelling and polymerization method. Based on this media, a new hydrophilic weak cation exchange stationary phase (WCX) for high performance liquid chromatography was synthesized by a new chemical modification method. The stationary phase was evaluated on the behavior of ion exchange, separability, and hydrophilicity. Effects of the nature of salts and pH value on the separation and retention of proteins of the stationary phase were investigated in details. It was found that the WCX resin follows ion exchange chromatographic retention mechanism. It was also used for the rapid separation and purification of lysozyme from egg white in only one step. The purity was found more than 96% and specific bioactivity of the purified lysozyme was as high as 71 184 U/mg.

  20. 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.

  1. Immobilization of Candida rugosa lipase on hydrophobic/strong cation-exchange functional silica particles for biocatalytic synthesis of phytosterol esters.

    PubMed

    Zheng, Ming-Ming; Lu, Yong; Dong, Ling; Guo, Ping-Mei; Deng, Qian-Chun; Li, Wen-Lin; Feng, Yu-Qi; Huang, Feng-Hong

    2012-07-01

    In this work, mixed-mode silica particles functionalized with octyl and sulfonic acid groups was conveniently prepared by co-bonding a mixture of n-octyltriethoxysilane and 3-mercaptopropyltriethoxysilane and then oxidized with hydrogen peroxide. Candida rugosa lipase (CRL) was immobilized on the mixed-mode silica particles via hydrophobic and strong cation-exchange interaction. The resulting immobilized CRL increased remarkably its stability at high temperature in comparison to free CRL. The immobilized CRL was used as biocatalysts for enzymatic esterification of phytosterols with free fatty acids (FFAs) to produce phytosterol esters. The phytosterols linolenate esterification degree of 95.3% was obtained under the optimized condition. Phytosterols esters could also been converted in high yields to the corresponding long-chain acyl esters via transesterification with methyl esters of fatty acids (80.5%) or triacylglycerols (above 95.5%) using mixed-mode silica particles immobilized CRL as biocatalyst. Furthermore, the immobilized CRL by absorption retained 78.6% of their initial activity after 7 recycles.

  2. Synthesis and application of hypercrosslinked polymers with weak cation-exchange character for the selective extraction of basic pharmaceuticals from complex environmental water samples.

    PubMed

    Bratkowska, D; Marcé, R M; Cormack, P A G; Sherrington, D C; Borrull, F; Fontanals, N

    2010-03-05

    The synthesis of high specific surface area sorbents (HXLPP-WCX) in the form of hypercrosslinked polymer microspheres with narrow particle size distributions, average particle diameters around 6 microm, and weak cation-exchange (WCX) character, is described. The WCX character arises from carboxylic acid moieties in the polymers, derived from the comonomer methacrylic acid. A novel HXLPP-WCX sorbent with an attractive set of chemical and physical properties was then used in an off-line solid-phase extraction (SPE) protocol for the selective extraction of a group of basic compounds from complex environmental samples, a priority being the clean separation of the basic compounds of interest from acidic compounds and interferences. The separation power of the new sorbent for basic pharmaceuticals was compared to two commercially available, mixed-mode sorbents, namely Oasis WCX and Strata-X-CW. Under identical experimental conditions, HXLPP-WCX was found to deliver both higher capacity and better selectivity in SPE than either of the two commercially available materials. In an optimised SPE protocol, the HXLPP-WCX sorbent gave rise to quantitative and selective extractions of low microg l(-1) levels of basic pharmaceuticals present in 500 ml of river water and 250 ml of effluent waste water.

  3. Low-capacity cation-exchange chromatography of amino acids using a novel sulfoacylated macroreticular polystyrene-divinylbenzene column with binary gradient elution.

    PubMed

    Yokoyama, Yukio; Wakabayashi, Natsuko; Furugaki, Yuki; Sato, Hisakuni

    2004-08-01

    This paper describes a versatile technique for amino-acid separation using a novel low-capacity sulfoacylated macroreticular polystyrene-divinylbenzene cation-exchange column with a simple binary high-pressure pH gradient elution. Proteinic 16 amino acids were well separated within 50 min using a H3PO4/Na2HPO4-CH3CN eluent system, and the cycle time was about 70 min. The chromatography with postcolumn OPA fluorescent detection was reproducible with RSDs less than 1% for retention times, and was quantitative with RSDs less than 5% for area responses. A linear regression line with an r2 value above 0.9990 was obtained for each analyte in concentration from 0.1 to 10 microM by 20 microL injection. The method was applicable to the separation and detection of urinary diagnostic amino acid due to inborn errors of metabolism, such as phenylketonuria. The analytical costs would be decreased by using the proposed method.

  4. 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/.

  5. Polypyrrole nanocomposite made by polypyrrole dispersion in poly (vinyl alcohol) matrix

    NASA Astrophysics Data System (ADS)

    Bhadra, J.; Sarkar, D.

    2010-10-01

    Polypyrrole-polyvinyl alcohol (PPy-PVA) nanocomposite is synthesized by dispersing interface polymerized polypyrrole in PVA matrix. The composite films are characterized by FTIR, XRD and SEM. FTIR spectra indicates crosslinking in the composite film. XRD pictures show more crystallinity for higher polymerization temperature, whereas SEM pictures clearly indicate PPy rod formation for the same film. The electrical conductivity of the films is in the range of 10-1 S/cm, whereas the current-voltage (I-V) characteristics shows power law behaviour.

  6. Facile synthesis of monodisperse functional magnetic dialdehyde starch nano-composite and used for highly effective recovery of Hg(II).

    PubMed

    Wang, Yang; Zhang, Yun; Hou, Chen; Qi, Zhigang; He, Xinghua; Li, Yanfeng

    2015-12-01

    By covalently linking dialdehyde starch and amine functionalized Fe3O4 nanoparticle, and modifying with aminothiourea functional group, the novel monodisperse nano-composite has been successfully synthesized without any toxic crosslinking agent. The resulting nano-composite was characterized by means of the Fourier transform infrared spectra (FT-IR), transmission electron microscope (TEM), X-ray diffraction (XRD), elemental analysis and vibrating sample magnetometer (VSM). As the new kind of low-cost and environmentally friendly adsorbent with the excellent monodispersity in aqueous phase, the obtained nano-composite has shown not only the good adsorption capacity for Hg(II) on high initial concentration, but also the strong removal ability on low concentration. Moreover, the unique selectivity for Hg(II) among the mixed metal ions solution and good regeneration performance of nano-composite has also been demonstrated by batch experiments.

  7. 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.

  8. Nano-composite scaffolds for bone tissue engineering containing silver nanoparticles: preparation, characterization and biological properties.

    PubMed

    Marsich, Eleonora; Bellomo, Francesca; Turco, Gianluca; Travan, Andrea; Donati, Ivan; Paoletti, Sergio

    2013-07-01

    In this study nano-composite scaffolds to be used as bone grafts have been endowed with antibacterial properties owing to the presence of silver nanoparticles. The alginate/hydroxyapatite composite scaffolds were prepared by internal gelation followed by a freeze-drying procedure to obtain a porous structure. The nanoparticles were prepared in presence of a lactose modified-chitosan and this colloidal solution was adsorbed on the scaffolds by exploiting electrostatic interactions. The adsorption and release of the silver from the composite scaffold was measured by ICP-AES and spectrofluorimetry measurements. Micro-computed tomography analysis of the scaffolds showed a homogeneous porous structure with average pore sizes of 341.5 μm and porosity of 80 %. In vitro biological tests (MTS and killing kinetics assays) demonstrated that silver does not affect the ability of the scaffolds to promote osteoblasts proliferation and that at the same time it exerts a strong bactericidal effect against both Gram+ and Gram- bacterial strains. Overall, the combined results indicate that these biocompatible antimicrobial scaffolds possess ideal characteristics for tissue engineering applications.

  9. 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.

  10. Thermal, mechanical and electrical properties of polyanaline based ceramic nano-composites

    NASA Astrophysics Data System (ADS)

    Sohail, M.; Khan, M. S.; Khattak, N. S.

    2016-08-01

    Micro/nanohybrid materials have vast applications due to their great potentialities in the field of nanoscience and nanotechnology. Herein we report an investigation on the fabrication and physicochemical characterization of ceramic (Fe0.01La0.01Al0.5Zn0.98O) and hybrid ceramic-polyaniline nano-composits. Ceramic nano-particles were prepared by sol-gel technique while optimizing the molar ratios of the constituent's metal nitrates. The prepared inorganic particles were then embedded in the polymer matrix via one-pot blending method. The prepared ceramic particles and their composites with polyaniline were analysed under FT- IR, SEM and TGA. The presence of some chemical species was observed at the interface of the compositing materials. TGA analysis showed the thermal stability of the composite material. Frequency dependent dielectric properties were analysed and it was found that conducting polyaniline has an additional effect on the electrical behaviour of the composite. Rheology study showed enhanced mechanical properties of composite material as compared to their constituting counterparts.

  11. Fabrication and mechanical evaluation of hydroxyapatite/oxide nano-composite materials.

    PubMed

    Mohamed, Khaled R; Beherei, Hanan H; El Bassyouni, Gehan T; El Mahallawy, Nahed

    2013-10-01

    In the current study, the semiconducting metal oxides such as nano-ZnO and SiO2 powders were prepared via sol-gel technique and conducted on nano-hydroxyapatite (nHA) which was synthesized by chemical precipitation. The properties of fabricated nano-structured composites containing different ratios of HA, ZnO and SiO2 were examined using X-ray diffraction (XRD), Fourier transform infrared (FT-IR) spectroscopy, scanning electron microscope (SEM) and transmission electron microscope (TEM) techniques. The effect of the variation of ratios between the three components on mechanical, microstructure and in-vitro properties was assessed to explore the possibility of enhancing these properties. The results proved that the mechanical properties exhibited an increment with increasing the ZnO content at the extent of HA. In-vitro study proved the formation and nucleation of apatite onto the surface of the fabricated composites after one week of immersion. It is concluded that HA composites containing SiO2 or SiO2/ZnO content had a suitable mechanical properties and ability to form apatite particles onto the composite surface. Based on bioactivity behavior, Si-HA is more bioactive than pure hydroxyapatite and nano-arrangements will provide an interface for better bone formation. Therefore, these nano-composites will be promising as bone substitutes especially in load bearing sites.

  12. One-pot synthesis of carbon-coated SnO2 nano-composite using hydrothermal method for lithium ion battery application.

    PubMed

    Lee, Hye Rim; Kim, Hwan Jin; Park, Jong Hyeok; Yoon, Dae Ho

    2013-06-01

    Carbon-coated SnO2 nano-composite was synthesized by using a hydrothermal method in a one step process with sizes of 1 to 3 microm. The carbon-coated SnO2 nano-composite was easily obtained by changing firing atmosphere from air to argon (600 degrees C for 3 hours). The carbon-coating thickness and size of the SnO2 nanoparticles in carbon-coated SnO2 nano-composite were confirmed through a high-resolution transmission electron microscopy (HRTEM) as 40 and 5 nm, respectively. Carbon-coating and particle size affect to the capacity retention property. Carbon-coated and non carbon-coated samples were investigated as anode materials. It was confirmed that the non carbon-coated SnO2 nano-composite had a 718 mA h/g initial charge capacity, 91% reached to theoretical value of SnO2 (790 mA h/g), while the carbon-coated SnO2 nano-composite had an excellent capacity retention of 89.6% after 70 cycles (10.88% for non carbon-coated SnO2 nano-composite).

  13. Determination of melamine and cyromazine in milk by high performance liquid chromatography coupled with online solid-phase extraction using a novel cation-exchange restricted access material synthesized by surface initiated atom transfer radical polymerization.

    PubMed

    Zhang, Yingying; Lin, Shen; Jiang, Ping; Zhu, Xudong; Ling, Jing; Zhang, Wen; Dong, Xiangchao

    2014-04-11

    A novel strong-cation-exchange restricted access material has been synthesized by atom transfer radical polymerization (ATRP). In the synthesis, poly(3-sulfopropyl methacrylate-co-ethylene dimethacrylate), [p(SPM/EDMA)] was grafted on the silica by surface-initiated ATRP first. The poly(glycerol mono-methacrylate) [pGMMA] was then immobilized on the external surface, which created a chemical diffusion barrier for protein exclusion. The resulting Sil-g-p(SPM/EDMA)-g-pGMMA has both functions of protein exclusion and cation exchange, exhibiting the property of cation-exchange restricted access material. The application of Sil-g-p(SPM/EDMA)-g-pGMMA has been studied by the determination of melamine and cyromazine in bovine milk using the online solid-phase extraction/HPLC method. In the process, the Sil-g-p(SPM/EDMA)-g-pGMMA was used for the sample pre-treatment and a HILIC column was employed as the analytical column. The method has shown good accuracy, precision and low limits of detections. The result demonstrated that the Sil-g-p(SPM/EDMA)-g-pGMMA can be used for the cation extraction from biological samples by direct HPLC injection.

  14. 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.

  15. Unfolding and aggregation of a glycosylated monoclonal antibody on a cation exchange column. Part I. Chromatographic elution and batch adsorption behavior.

    PubMed

    Guo, Jing; Zhang, Shaojie; Carta, Giorgio

    2014-08-22

    A glycosylated IgG2 monoclonal antibody exhibits a two-peak elution behavior when loaded on a strong cation exchange column and eluted with either a linear salt gradient or two salt steps at increasing salt concentrations. The two-peak behavior is more pronounced for conditions where the initial antibody binding is stronger, i.e. at lower pH and buffer concentration, where the hold time prior to elution is longer, where the protein mass load is lower, and where the load flow rate is higher. The effect is also dependent on the resin type, being prominent for the polymer-functionalized resin Fractogel EMD SO₃(-) and virtually absent for a macroporous resin with similar backbone but no grafted polymers. Size exclusion chromatography and dynamic light scattering show that the early eluting peak consists exclusively of the native monomeric species while the late eluting peak is a mixture of monomeric and aggregated species. Batch adsorption/desorption experiments show that the bound protein can be desorbed in two steps, with a fraction desorbed in 0.33 M NaCl, corresponding to native monomer, and a second fraction desorbed in 1M NaCl. The latter fraction decreases with protein mass load and becomes almost negligible when the resin is initially completely saturated with protein. Confocal laser scanning microscopy showed that the two-peak elution/desorption behavior is related to the unique kinetics of protein binding in the Fractogel resin. Following partial loading of the resin, the bound protein migrates toward the center of the particles during a hold step and is redistributed across the particle volume attaining low local bound protein concentrations. For these conditions the protein is apparently destabilized forming a strongly-bound unfolded intermediate that, in turn, generates aggregates upon elution in high salt.

  16. Removal of copper(II) from aqueous phase by Purolite C100-MB cation exchange resin in fixed bed columns: modeling.

    PubMed

    Hamdaoui, Oualid

    2009-01-30

    The dynamic removal of copper by Purolite C100-MB cation exchange resin was studied in packed bed columns. The values of column parameters are predicted as a function of flow rate and bed height. Batch experiments were performed using the Na-form resin to determine equilibrium and kinetics of copper removal. The uptake of Cu(II) by this resin follows first-order kinetics. The effect of stirring speed and temperature on the removal kinetics was studied. The activation energy for the exchange reaction is 13.58kJmol(-1). The equilibrium data obtained in this study have been found to fit both the Langmuir and Freundlich isotherm equations. A series of column tests were performed to determine the breakthrough curves with varying bed heights and flow rates. To predict the breakthrough curves and to determine the characteristic parameters of the column useful for process design, four kinetic models; Bohart-Adams, Bed Depth Service Time (BDST), Clark and Wolborska models are applied to experimental data. All models are found suitable for describing the whole or a definite part of the dynamic behavior of the column with respect to flow rate and bed height. The simulation of the whole breakthrough curve is effective with the Bohart-Adams and the Clark models, but the Bohart-Adams model is better. The breakthrough is best predicted by the Wolborska model. The breakthrough data gave a good fit to the BDST model, resulting in a bed exchange capacity very close to the value determined in the batch process.

  17. Monoclonal antibody heterogeneity analysis and deamidation monitoring with high-performance cation-exchange chromatofocusing using simple, two component buffer systems.

    PubMed

    Kang, Xuezhen; Kutzko, Joseph P; Hayes, Michael L; Frey, Douglas D

    2013-03-29

    The use of either a polyampholyte buffer or a simple buffer system for the high-performance cation-exchange chromatofocusing of monoclonal antibodies is demonstrated for the case where the pH gradient is produced entirely inside the column and with no external mixing of buffers. The simple buffer system used was composed of two buffering species, one which becomes adsorbed onto the column packing and one which does not adsorb, together with an adsorbed ion that does not participate in acid-base equilibrium. The method which employs the simple buffer system is capable of producing a gradual pH gradient in the neutral to acidic pH range that can be adjusted by proper selection of the starting and ending pH values for the gradient as well as the buffering species concentration, pKa, and molecular size. By using this approach, variants of representative monoclonal antibodies with isoelectric points of 7.0 or less were separated with high resolution so that the approach can serve as a complementary alternative to isoelectric focusing for characterizing a monoclonal antibody based on differences in the isoelectric points of the variants present. Because the simple buffer system used eliminates the use of polyampholytes, the method is suitable for antibody heterogeneity analysis coupled with mass spectrometry. The method can also be used at the preparative scale to collect highly purified isoelectric variants of an antibody for further study. To illustrate this, a single isoelectric point variant of a monoclonal antibody was collected and used for a stability study under forced deamidation conditions.

  18. 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.

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

    PubMed

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

    2015-10-09

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

  20. 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.

  1. 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.

  2. 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

  3. 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

  4. 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.

  5. 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.

  6. 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.

  7. Electrochemical polypyrrole formation from pyrrole 'adlayer'.

    PubMed

    Plausinaitis, Deivis; Sinkevicius, Linas; Mikoliunaite, Lina; Plausinaitiene, Valentina; Ramanaviciene, Almira; Ramanavicius, Arunas

    2017-01-04

    In this research study, we investigated the morphology of polypyrrole nanostructures, which were formed during the electrochemical deposition of conducting polymer. An electrochemical quartz crystal microbalance (EQCM) cell equipped with a flow-through system was employed to exchange solutions of different compositions within the EQCM cell. When bare PBS buffer in the EQCM cell was exchanged with PBS buffer with pyrrole we observed a distinct increase in the resonance frequency Δf. This change in the resonance frequency and electrical capacitance, which was calculated from electrochemical impedance spectroscopy (EIS) data, illustrate that pyrrole on the surface of the gold electrode formed an adsorbed layer (adlayer). The formation of a pyrrole adlayer before the potential pulse that induced polymerization was investigated by QCM-based measurements. The electrochemical polymerization of this adlayer was induced by a single potential pulse and a nanostructured layer, which consisted of adsorbed polypyrrole (Ppy) nanoparticles with a diameter of 50 nm, was formed. QCM and EIS data revealed that by the next cycle of the electrochemical formation of Ppy, which was investigated after flow-through-based exchange of solutions, the initially formed Ppy surface was covered by the adlayer of pyrrole. This adlayer was desorbed when pyrrole was removed from the solution. When electrochemical polymerization was performed using 50 potential pulses, a Ppy layer, which had more complex morphology, was formed on the EQCM crystal. Scanning electron microscopy showed that the conductivity of this layer was unequally distributed. We observed that the polypyrrole layer formed by electrochemical deposition, which was performed using potential pulses, was formed out of aggregated spherical Ppy particles with a diameter of 50 nm.

  8. Polyaniline-polypyrrole composites with enhanced hydrogen storage capacities.

    PubMed

    Attia, Nour F; Geckeler, Kurt E

    2013-06-13

    A facile method for the synthesis of polyaniline-polypyrrole composite materials with network morphology is developed based on polyaniline nanofibers covered by a thin layer of polypyrrole via vapor phase polymerization. The hydrogen storage capacity of the composites is evaluated at room temperature exhibits a twofold increase in hydrogen storage capacity. The HCl-doped polyaniline nanofibers exhibit a storage capacity of 0.46 wt%, whereas the polyaniline-polypyrrole composites could store 0.91 wt% of hydrogen gas. In addition, the effect of the dopant type, counteranion size, and the doping with palladium nanoparticles on the storage properties are also investigated.

  9. Nanostructured Polypyrrole-Based Ammonia and Volatile Organic Compound Sensors

    PubMed Central

    Šetka, Milena; Drbohlavová, Jana; Hubálek, Jaromír

    2017-01-01

    The aim of this review is to summarize the recent progress in the fabrication of efficient nanostructured polymer-based sensors with special focus on polypyrrole. The correlation between physico-chemical parameters, mainly morphology of various polypyrrole nanostructures, and their sensitivity towards selected gas and volatile organic compounds (VOC) is provided. The different approaches of polypyrrole modification with other functional materials are also discussed. With respect to possible sensors application in medicine, namely in the diagnosis of diseases via the detection of volatile biomarkers from human breath, the sensor interaction with humidity is described as well. The major attention is paid to analytes such as ammonia and various alcohols. PMID:28287435

  10. Nanostructured Polypyrrole-Based Ammonia and Volatile Organic Compound Sensors.

    PubMed

    Šetka, Milena; Drbohlavová, Jana; Hubálek, Jaromír

    2017-03-10

    The aim of this review is to summarize the recent progress in the fabrication of efficient nanostructured polymer-based sensors with special focus on polypyrrole. The correlation between physico-chemical parameters, mainly morphology of various polypyrrole nanostructures, and their sensitivity towards selected gas and volatile organic compounds (VOC) is provided. The different approaches of polypyrrole modification with other functional materials are also discussed. With respect to possible sensors application in medicine, namely in the diagnosis of diseases via the detection of volatile biomarkers from human breath, the sensor interaction with humidity is described as well. The major attention is paid to analytes such as ammonia and various alcohols.

  11. Gold surface supported spherical liposome-gold nano-particle nano-composite for label free DNA sensing.

    PubMed

    Bhuvana, M; Narayanan, J Shankara; Dharuman, V; Teng, W; Hahn, J H; Jayakumar, K

    2013-03-15

    Immobilization of 1,2-dioleoyl-sn-glycero-3-phosphoethanolamine (DOPE) liposome-gold nano-particle (DOPE-AuNP) nano-composite covalently on 3-mercaptopropionic acid (MPA) on gold surface is demonstrated for the first time for electrochemical label free DNA sensing. Spherical nature of the DOPE on the MPA monolayer is confirmed by the appearance of sigmoidal voltammetric profile, characteristic behavior of linear diffusion, for the MPA-DOPE in presence of [Fe(CN)(6)](3-/4-) and [Ru(NH(3))(6)](3+) redox probes. The DOPE liposome vesicle fusion is prevented by electroless deposition of AuNP on the hydrophilic amine head groups of the DOPE. Immobilization of single stranded DNA (ssDNA) is made via simple gold-thiol linkage for DNA hybridization sensing in the presence of [Fe(CN)(6)](3-/4-). The sensor discriminates the hybridized (complementary target hybridized), un-hybridized (non-complementary target hybridized) and single base mismatch target hybridized surfaces sensitively and selectively without signal amplification. The lowest target DNA concentration detected is 0.1×10(-12)M. Cyclic voltammetry (CV), electrochemical impedance (EIS), differential pulse voltammetry (DPV) and quartz crystal microbalance (QCM) techniques are used for DNA sensing on DOPE-AuNP nano-composite. Transmission Electron Microscopy (TEM), Fourier Transform Infrared Spectroscopy (FTIR), Atomic Force Microscopy (AFM), Dynamic Light Scattering (DLS) and Ultraviolet-Visible (UV) spectroscopic techniques are used to understand the interactions between the DOPE, AuNP and ssDNA. The results indicate the presence of an intact and well defined spherical DOPE-AuNP nano-composite on the gold surface. The method could be applied for fabrication of the surface based liposome-AuNP-DNA composite for cell transfection studies at reduced reagents and costs.

  12. A novel cation exchange polymer as a reversed-dispersive solid phase extraction sorbent for the rapid determination of rhodamine B residue in chili powder and chili oil.

    PubMed

    Chen, Dawei; Zhao, Yunfeng; Miao, Hong; Wu, Yongning

    2014-12-29

    This paper presents a new analytical method for the determination of rhodamine B (RB) residue in chili powder and chili oil based on a novel reversed-dispersive solid phase extraction (r-dSPE) and ultra high performance liquid chromatography–high resolution mass spectrometry (UHPLC–HRMS). Chili powder and chili oil samples were first extracted with acetonitrile/water (1:1, v/v) and acetonitrile, respectively. Then, RB from the extract was adsorbed to the polymer cation exchange (PCX) sorbent with the characteristics of ion exchange and reversed-phase retention. Subsequently, the analyte in PCX sorbent was eluted with ammonium hydroxide/methanol (1:99, v/v) through a simple unit device equipped with 1 mL syringe and 0.22 μm nylon syringe filter. All of the samples were analyzed by UHPLC–HRMS/MS on a Waters Acquity BEH C18 column with 0.1% formic acid and 4 mM ammonium formate in water/acetonitrile as the mobile phase with gradient elution. The matrix effect, recovery, and repeatability, within laboratory reproducibility, and the LODs and LOQs of the r-dSPE cleanup method were investigated. The method showed a good linearity (R2 > 0.999) in the ranges of 0.01–1 μg/L and 1–100 μg/L for the analyte. The LODs of RB for chili powder and chili oil samples were 0.5 μg/kg. The average recoveries of RB from the samples spiked at four different concentrations (2, 20, 500 and 5000 μg/kg) were in a range from 76.7 to 104.9%. Results showed that the proposed method was simple, fast, economical and effective for the determination of RB in chili powder and chili oil. Considering the excellent sorptive performance of PCX for RB, further work should be done to evaluate the usefulness of the PCX in r-dSPE for the clean-up and analyses of other trace-level alkaline contaminants.

  13. Influence of the water content on the diffusion coefficients of Li+ and water across naphthalenic based copolyimide cation-exchange membranes.

    PubMed

    Garrido, Leoncio; Pozuelo, Javier; López-González, Mar; Yan, Gengwei; Fang, Jianhua; Riande, Evaristo

    2012-09-27

    The transport of lithium ions in cation-exchange membranes based on sulfonated copolyimide membranes is reported. Diffusion coefficients of lithium are estimated as a function of the water content in membranes by using pulsed field gradient (PFG) NMR and electrical conductivity techniques. It is found that the lithium transport slightly decreases with the diminution of water for membranes with water content lying in the range 14 < λ < 26.5, where λ is the number of molecules of water per fixed sulfonate group. For λ < 14, the value of the diffusion coefficient of lithium experiences a sharp decay with the reduction of water in the membranes. The dependence of the diffusion of lithium on the humidity of the membranes calculated from conductivity data using Nernst-Planck type equations follows a trend similar to that observed by NMR. The possible explanation of the fact that the Haven ratio is higher than the unit is discussed. The diffusion of water estimated by (1)H PFG-NMR in membranes neutralized with lithium decreases as λ decreases, but the drop is sharper in the region where the decrease of the diffusion of protons of water also undergoes considerable reduction. The diffusion of lithium ions computed by full molecular dynamics is similar to that estimated by NMR. However, for membranes with medium and low concentration of water, steady state conditions are not reached in the computations and the diffusion coefficients obtained by MD simulation techniques are overestimated. The curves depicting the variation of the diffusion coefficient of water estimated by NMR and full dynamics follow parallel trends, though the values of the diffusion coefficient in the latter case are somewhat higher. The WAXS diffractograms of fully hydrated membranes exhibit the ionomer peak at q = 2.8 nm(-1), the peak being shifted to higher q as the water content of the membranes decreases. The diffractograms present additional peaks at higher q, common to wet and dry membranes, but

  14. 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

  15. Process development for robust removal of aggregates using cation exchange chromatography in monoclonal antibody purification with implementation of quality by design.

    PubMed

    Xu, Zhihao; Li, Jason; Zhou, Joe X

    2012-01-01

    Aggregate removal is one of the most important aspects in monoclonal antibody (mAb) purification. Cation-exchange chromatography (CEX), a widely used polishing step in mAb purification, is able to clear both process-related impurities and product-related impurities. In this study, with the implementation of quality by design (QbD), a process development approach for robust removal of aggregates using CEX is described. First, resin screening studies were performed and a suitable CEX resin was chosen because of its relatively better selectivity and higher dynamic binding capacity. Second, a pH-conductivity hybrid gradient elution method for the CEX was established, and the risk assessment for the process was carried out. Third, a process characterization study was used to evaluate the impact of the potentially important process parameters on the process performance with respect to aggregate removal. Accordingly, a process design space was established. Aggregate level in load is the critical parameter. Its operating range is set at 0-3% and the acceptable range is set at 0-5%. Equilibration buffer is the key parameter. Its operating range is set at 40 ± 5 mM acetate, pH 5.0 ± 0.1, and acceptable range is set at 40 ± 10 mM acetate, pH 5.0 ± 0.2. Elution buffer, load mass, and gradient elution volume are non-key parameters; their operating ranges and acceptable ranges are equally set at 250 ± 10 mM acetate, pH 6.0 ± 0.2, 45 ± 10 g/L resin, and 10 ± 20% CV respectively. Finally, the process was scaled up 80 times and the impurities removal profiles were revealed. Three scaled-up runs showed that the size-exclusion chromatography (SEC) purity of the CEX pool was 99.8% or above and the step yield was above 92%, thereby proving that the process is both consistent and robust.

  16. Preparation of a novel weak cation exchange/hydrophobic interaction chromatography dual-function polymer-based stationary phase for protein separation using "thiol-ene click chemistry".

    PubMed

    Yang, Fan; Bai, Quan; Zhao, Kailou; Gao, Dong; Tian, Lei

    2015-02-01

    A novel dual-function mixed-mode stationary phase based on poly(glycidyl methacrylate-co-ethylene dimethacrylate) microspheres was synthesized by thiol-ene click chemistry and characterized by infrared spectroscopy and elemental analysis. The new system displays both hydrophobic interaction chromatography (HIC) character in a high salt concentration mobile phase, and weak cation exchange (WCX) chromatography character in a low salt concentration mobile phase. It can be used to separate proteins in both ion-exchange chromatography (IEC) mode and HIC mode. The resolution and selectivity of the stationary phase were evaluated in both HIC mode and IEC mode using protein standards. In comparison with the conventional WCX and HIC columns, the results were satisfactory and acceptable. Protein mass and bioactivity recoveries of more than 96% can be achieved in both HIC mode and IEC mode using this column. The results indicate that the novel dual-function mixed-mode column in many cases can replace the use of two individual WCX and HIC columns. In addition, the effects on protein separation of different ligand structures in the dual-function stationary phase and the pH of the mobile phase used were also investigated in detail. The results show that electrostatic interaction of the ligand with proteins must match the hydrophobicity of the ligand, which is an important factor to prepare the dual-function stationary phase. On the basis of this dual-function mixed-mode chromatography column, a new two-dimensional liquid chromatography technology with a single column system was also developed in this study, and was used to renature and purify recombinant human interferon-γ from inclusion bodies. The mass recovery, purity, and specific bioactivity obtained for the purified recombinant human interferon-γ were 87.2%, 92.4%, and 2.8 × 10(7) IU/mg, respectively, in IEC mode, and 83.4%, 95.2%, and 4.3 × 10(7) IU/mg, respectively, in HIC mode. The results indicate that the

  17. Structural and magnetic characteristics of PVA/CoFe{sub 2}O{sub 4} nano-composites prepared via mechanical alloying method

    SciTech Connect

    Rashidi, S.; Ataie, A.

    2016-08-15

    Highlights: • Single phase CoFe{sub 2}O{sub 4} nano-particles synthesized in one step by mechanical alloying. • PVA/CoFe{sub 2}O{sub 4} magnetic nano-composites were fabricated via mechanical milling. • FTIR confirmed the interaction between PVA and magnetic CoFe{sub 2}O{sub 4} particles. • Increasing in milling time and PVA amount led to well dispersion of CoFe{sub 2}O{sub 4}. - Abstract: In this research, polyvinyl alcohol/cobalt ferrite nano-composites were successfully synthesized employing a two-step procedure: the spherical single-phase cobalt ferrite of 20 ± 4 nm mean particle size was synthesized via mechanical alloying method and then embedded into polymer matrix by intensive milling. The results revealed that increase in polyvinyl alcohol content and milling time causes cobalt ferrite particles disperse more homogeneously in polymer matrix, while the mean particle size and shape of cobalt ferrite have not been significantly affected. Transmission electron microscope images indicated that polyvinyl alcohol chains have surrounded the cobalt ferrite nano-particles; also, the interaction between polymer and cobalt ferrite particles in nano-composite samples was confirmed. Magnetic properties evaluation showed that saturation magnetization, coercivity and anisotropy constant values decreased in nano-composite samples compared to pure cobalt ferrite. However, the coercivity values of related nano-composite samples enhanced by increasing PVA amount due to domain wall mechanism.

  18. 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.

  19. Incorporation of pyrene in polypyrrole/polystyrene magnetic beads.

    PubMed

    Głowala, Paulina; Budniak, Adam; Krug, Pamela; Wysocka, Barbara; Berbeć, Sylwia; Dec, Robert; Dołęga, Izabela; Kacprzak, Kamil; Wojciechowski, Jarosław; Kawałko, Jakub; Kępka, Paweł; Kępińska, Daria; Kijewska, Krystyna; Mazur, Maciej

    2014-10-15

    Pyrene, a fluorescent dye, was incorporated into polystyrene particles coated with polypyrrole. The incorporation was achieved by treating the polypyrrole/polystyrene (PPy/PS) beads in a tetrahydrofuran (THF) solution of the pyrene fluorophore followed by rinsing with methanol. The polystyrene cores of the beads swell in THF, allowing penetration of pyrene molecules into the polystyrene structure. The addition of methanol causes contraction of the swollen polystyrene, which encapsulates the dye molecules inside the beads. It is shown that the polypyrrole coating is permeable with respect to both the dye and the solvent, allowing the transport of molecules between the polystyrene cores and the contacting solution. The polypyrrole adlayer can be used as a matrix for the incorporation of magnetic nanoparticles. Embedded particles provide magnetic functionality to the PPy/PS beads. It is demonstrated that the pyrene-loaded beads can be manipulated with an external magnetic field.

  20. 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.

  1. 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.

  2. Improvement of hydrophilic property of rubber dipping former surface with Ni/B/TiO2 nano-composite film

    NASA Astrophysics Data System (ADS)

    Sikong, L.; Masae, M.; Kooptarnond, K.; Taweepreda, W.; Saito, F.

    2012-03-01

    The objective of this study is to explore a method to improve hydrophilicity of the surface of formers that could be more easily dipped to produce high quality dipped rubber products. Photocatalytic TiO2 composite films were prepared by sol-gel method. Glass formers were coated with the Ni/B/TiO2 nano-composite film by dipping method and annealed at 400 °C for 1 h. Phase formation of TiO2 was characterized by XRD. Morphology of the TiO2 films was observed by using atomic force microscopy (AFM). Optical absorption of the films and degradation concentration of methylene blue had been measured employing UV-vis spectrophotometer. The hydrophilicity of the thin films was determined in terms of the contact angles of water and NR rubber latex droplets on the coated TiO2 composite films with and without UV irradiation. It was found from the experimental study that the Ni/B/TiO2 nano-composite film can improve wet-ability of the coated former surfaces, leading to enhancement of tensile strengths of the vulcanized natural rubber (NR) latex films.

  3. 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.

  4. A study of thermal spray coated surface with nano composite powder of CNT+WC14C0

    NASA Astrophysics Data System (ADS)

    Balan, K. N.; Valarmathi, T. N.; Nuttaki, Akhil; Sai Vivek Reddy, Arani; Sai Srinivas, Jammalamadaka K. M. K.; Nathanael, M. Antony

    2016-09-01

    Coatings obtained from thermal spray process are being developed for wide varieties of applications in aerospace and automotive industries. To enhance the wear resistance in the YAWING in wind mills, a new study is required to find out and analyze the surface properties of the surface of Yawing. In this study to enhance the surface properties, a new nano composite powder has been developed and coated on SS304. To synthesis of CNT+WC14Co, initially a binder material of 0.5% Poly Vinyl alcohol solution was prepared and made use as a binder between CNT and WC14Co particles. The synthesized nano composite powder is coated over SS304 samples as per Taguchi design of experiments by Detonation gun coating technique. The coated samples are undergone the tests of micro hardness and Surface roughness. It was found that a significant improvement in micro hardness and there is no significant improvement in surface finish. The best combination of input parameters is obtained through Taguchi method and untried combination's results also have been predicted through Taguchi method. Response surface methodology (RSM) is used to develop a mathematical model.

  5. 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

  6. 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.

  7. 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.

  8. 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.

  9. Multi-cycle recovery of lactoferrin and lactoperoxidase from crude whey using fimbriated high-capacity magnetic cation exchangers and a novel "rotor-stator" high-gradient magnetic separator.

    PubMed

    Brown, Geoffrey N; Müller, Christine; Theodosiou, Eirini; Franzreb, Matthias; Thomas, Owen R T

    2013-06-01

    Cerium (IV) initiated "graft-from" polymerization reactions were employed to convert M-PVA magnetic particles into polyacrylic acid-fimbriated magnetic cation exchange supports displaying ultra-high binding capacity for basic target proteins. The modifications, which were performed at 25 mg and 2.5 g scales, delivered maximum binding capacities (Qmax ) for hen egg white lysozyme in excess of 320 mg g(-1) , combined with sub-micromolar dissociation constants (0.45-0.69 µm) and "tightness of binding" values greater than 49 L g(-1) . Two batches of polyacrylic acid-fimbriated magnetic cation exchangers were combined to form a 5 g pooled batch exhibiting Qmax values for lysozyme, lactoferrin, and lactoperoxidase of 404, 585, and 685 mg g(-1) , respectively. These magnetic cation exchangers were subsequently employed together with a newly designed "rotor-stator" type HGMF rig, in five sequential cycles of recovery of lactoferrin and lactoperoxidase from 2 L batches of a crude sweet bovine whey feedstock. Lactoferrin purification performance was observed to remain relatively constant from one HGMF cycle to the next over the five operating cycles, with yields between 40% and 49% combined with purification and concentration factors of 37- to 46-fold and 1.3- to 1.6-fold, respectively. The far superior multi-cycle HGMF performance seen here compared to that observed in our earlier studies can be directly attributed to the combined use of improved high capacity adsorbents and superior particle resuspension afforded by the new "rotor-stator" HGMS design.

  10. Mechanical and thermal properties and morphological studies of 10 MeV electron beam irradiated LDPE/hydroxyapatite nano-composite

    NASA Astrophysics Data System (ADS)

    Soltani, Z.; Ziaie, F.; Ghaffari, M.; Afarideh, H.; Ehsani, M.

    2013-02-01

    In this work the nano-composite samples were prepared using the LDPE filled with different weight percentages of hydroxyapatite powder which was synthesized via hydrolysis method. The samples were subjected to irradiation under 10 MeV electron beam in 75-250 kGy doses. Mechanical and thermal properties as well as the morphology of the nano-composite samples were investigated and compared. The hot-set and swelling tests confirmed the radiation crosslinking induced in the polymer matrix especially between the matrix and reinforcement phase. The result indicates that the mechanical and thermal parameters are strongly dependent on the hydroxyapatite content in comparison to radiation.

  11. Development of separation technology for the removal of radium-223 from targeted thorium conjugate formulations. Part I: purification of decayed thorium-227 on cation exchange columns.

    PubMed

    Frenvik, Janne Olsen; Dyrstad, Knut; Kristensen, Solveig; Ryan, Olav B

    2017-02-01

    Targeted thorium conjugates (TTCs) are being explored as a potential future platform for specific tumor targeting pharmaceuticals. In TTCs, the alpha emitting radionuclide thorium-227 ((227)Th) with a half-life of 18.697 d is labeled to targeting moieties, such as monoclonal antibodies (mAbs). The amount of daughter nuclide radium-223 ((223)Ra, t1/2 = 11.435 d) will increase during manufacture and distribution, and so a technology for purification is required to assure an acceptable level of (223)Ra is administrated to the patient. Since (223)Ra is the only progeny of (227)Th with a long half-life (days), the progenies of (223)Ra will have a very limited stay in the formulation once (223)Ra is removed. The focus in this study has, therefore, been on the removal of (223)Ra. In this study, the sorption and separation of (223)Ra (radium(II)) and (227)Th (thorium(IV)) on cation exchange columns has been evaluated as a purification method of decayed (227)Th (i.e. prior to radiolabelling of a mAb and formation of TTC). The goal is to minimize the sorption of (227)Th and maximize the sorption of (223)Ra. Statistical experimental design with formulation and process parameters, including buffered formulations comprising citrate and acetate, at various concentrations and pH, presence of free radical scavenger and chelator, and resin amount have been evaluated for impact on the purification process. The studies have been interpreted by the aid of multivariate data analysis. The correlations between design of experimental variables and sorption are summarized by regression models. The predictive accuracy of radionuclide sorption was given by standard deviation and 95% confidence intervals originating from statistical cross validation. Experimental results and statistical models for citrate-buffered formulations verified reproducible and acceptable sorption levels of (223)Ra and (227)Th under selected conditions. For acetate-buffered formulations, prediction of (227)Th

  12. 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.

  13. 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.

  14. 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.

  15. Novel rare earth ions-doped oxyfluoride nano-composite with efficient upconversion white-light emission

    NASA Astrophysics Data System (ADS)

    Chen, Daqin; Wang, Yuansheng; Yu, Yunlong; Huang, Ping; Weng, Fangyi

    2008-10-01

    Transparent SiO 2-Al 2O 3-NaF-YF 3 bulk nano-composites triply doped with Ho 3+, Tm 3+ and Yb 3+ were fabricated by melt-quenching and subsequent heating. X-ray diffraction and transmission electron microscopy measurements demonstrated the homogeneous precipitation of the β-YF 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 3+ to Ho 3+ or Tm 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%.

  16. Preparation of magnetic nano-composite: barium hexaferrite loaded in the ordered meso-porous silica matrix (MCM-41).

    PubMed

    Emamian, H R; Honarbakhsh-Raouf, A; Ataie, A

    2010-04-01

    In this work a magnetic nano-composite was synthesized by modified incorporation of iron-barium complex into ordered meso-porous silica (MCM-41) as a matrix. The MCM-41 was synthesized by silylation treatment which was accompanied by pH adjusting. Low angle XRD patterns of both annealed MCM-41 and resulted composite exhibited the characteristic reflection of high quality hexagonal meso-structures. TEM image of the composite material revealed that the hexagonal ordered meso-structure host material was not affected by wet impregnation and subsequent calcination in order to incorporate with barium hexaferrite. Also, TEM images accompanied by EDS analysis confirmed the formation of second phase consists of barium and iron ions inside the MCM-41 channels. The resulted composite material showed a super-paramagnetic nature at room temperature.

  17. 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

  18. 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.

  19. 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

  20. 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.

  1. Ab-initio study of polypyrrole as a pervaporation membrane

    NASA Astrophysics Data System (ADS)

    Botelho, Andre; Lin, Xi

    2010-03-01

    The affinities between polypyrrole, water, ethanol and a sulfonate-carrying ion were calculated from first principles. All interactions were demonstrably hydrogen bonds between the oxygen from the sulfonate groups and the hydrogen in the hydroxyl (for water and ethanol) and amine groups (for polypyrrole). Each sulfonate group was shown to form three hydrogen bonds, with any of the three other types of molecules, allowing the ion complex to bind to multiple polypyrrole chains, water, and ethanol molecules simultaneously. The energies indicated a higher affinity between the ion and poypyrrole, second highest between water and the ion, and the lowest for ethanol and the ion. A high affinity of the ion to the polymer backbone is desirable to prevent leeching. The ion was found to have a higher affinity to water molecules than to ethanol, confirming the system's selectivity in separating water from ethanol.

  2. 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.

  3. Polypyrrole membranes as scaffolds for biomolecule immobilization

    NASA Astrophysics Data System (ADS)

    Hery, Travis M.; Satagopan, Sriram; Northcutt, Robert G.; Tabita, F. Robert; Sundaresan, Vishnu-Baba

    2016-12-01

    Enzymes have evolved over hundreds of years through changes in ecosystems (climate, atmosphere, hydrology, etc). The evolutionary changes driven by the need to survive has led to enzymes with diverse functionality such as reduction of carbon dioxide and methane to other forms of carbon, fixation of nitrogen, and high temperature biochemical processes. While these enzymes have useful properties, engineering a scalable cell-free system with these enzymes will be useful for stable production of desired products without involving the vagaries of cellular metabolism. This article presents various approaches to incorporate ribulose-1,5-bisphosphate carboxylase/oxygenase (RuBisCO) in a conducting polymer (polypyrrole (PPy)) doped with a bulky anion (dodecylbenzenesulfonate (DBS)) in an effort to create functional devices for the conversion of carbon dioxide into precursors for high-value chemicals. We demonstrate that the tailored device creates an environment where the enzyme can retain its function while being protected from denaturing conditions. It is envisioned that the 3-PGA produced by RuBisCO will be converted into value-added products.

  4. 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.

  5. 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.

  6. Column chromatographic separation of Hg(II), La(III), Ce(III), and In(III) from other metal ions in NH/sub 4/Cl-CH/sub 3/COOH medium by cation exchange

    SciTech Connect

    Srivastava, U.; Mahan, A.; Ghose, A.K.; Dey, A.K.

    1980-01-01

    Cation exchange equilibrium distribution coefficients (K) with the (Dowex 50W-X8) H/sup +/ form have been determined for 21 metal ions in media consisting of mixtures of 0.7 mol/dm/sup 3/ acetic acid and varying concentrations (0.16, 0.32, 0.48, 0.64, 0.96, and 1.28 mol/dm/sup 3/) of ammonium chloride. The distribution coefficients were determined by the batch technique for finding the conditions for the mentioned separations. The column chromatographic separations achieved were all quantitative. The results of the resolution of the synthetic binary and ternary mixtures along with the elution curves are presented. 3 figures, 4 tables.

  7. 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.

  8. Physicochemical study of the acetonitrile insertion into polypyrrole films.

    PubMed

    Oliveira Costa, S D; Fernández Romero, A J; López Cascales, J J

    2010-04-14

    A study by molecular dynamics (MD) simulation of the acetonitrile diffusion into a polypyrrole film was carried out with atomic detail in a 0.1N lithium perchlorate solution. From the simulated trajectories, the acetonitrile behavior was estimated from bulk solution to the interior of the polypyrrole film, across the polypyrrole/solution interface, for a neutral (reduced) and charged (oxidized) state of the polymer. Among other properties, the translational diffusion coefficient and rotational relaxation time of the acetonitrile were calculated, where a diminution in the translational diffusion coefficient was measured in the interior of the polypyrrole matrix compared to bulk, independently of the oxidation state of the polymer, in contrast with the behavior of the rotational relaxation time that increases from bulk to the interior of the polymer for both oxidation states. In addition, the difference of free energy DeltaG associated to the acetonitrile penetration into the polymer was calculated. From the results, it was evidenced that the scarce affinity of acetonitrile to diffuse into the polymer in its reduced state is related with the positive uniform difference of free energy DeltaG approximately 20 kJ/mol, while in the oxidized state, an important free energy barrier of DeltaG approximately 10 kJ/mol has to pass trough for reaching stable sites inside the polymer with values of DeltaG up to -10 kJ/mol.

  9. 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...

  10. 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

  11. Fabrication and characterization of cytocompatible polypyrrole films inkjet printed from nanoformulations cytocompatible, inkjet-printed polypyrrole films.

    PubMed

    Weng, Bo; Liu, Xiao; Higgins, Michael J; Shepherd, Roderick; Wallace, Gordon

    2011-12-16

    Inkjet printed polypyrrole (PPy) films with good uniformity and conductivity are fabricated from a stable, printable PPy nanodispersion, and the cytocompatability of these platforms is demonstrated using PC12 cells. This novel approach to fabricating PPy electrodes and films for tissue engineering and cell stimulation is particularly useful where microstructures are required.

  12. 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.

  13. 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.

  14. Preparation and characterization of poly(vinylidene fluoride): A high dielectric performance nano-composite for electrical storage

    NASA Astrophysics Data System (ADS)

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

    We have prepared films of polymer nano-composite (PNC) of poly[vinylidene-fluoride] (PVDF) and bismuth vanadate (BiVO4) nanoparticles. The α and γ electro-active phases were detected, and the addition of BiVO4 drastically increases the formation of the α-phase. Addition of BiVO4 produces up to 98% of electro-active phases. Robust electrostatic interactions arise between charges at the BiVO4-surfaces, and differences in electron affinity between CH2 and CF2 groups created dielectric dipoles. The addition of BiVO4 has not only enhanced the formation of the electrically active phases but also makes each dipole in the phase has its specific characteristics for example its own relaxation time. The AC-electrical permittivity showed that the dielectric constant of 10%wt- BiVO4 nanoparticles in PVDF has a value 44 ε0, which is four times more than the dielectric constant of the as-prepared PVDF films. These data show the importance of these polymers as easy, flexible, and durable energy storage materials.

  15. Creatinine and urea biosensors based on a novel ammonium ion-selective copper-polyaniline nano-composite.

    PubMed

    Zhybak, M; Beni, V; Vagin, M Y; Dempsey, E; Turner, A P F; Korpan, Y

    2016-03-15

    The use of a novel ammonium ion-specific copper-polyaniline nano-composite as transducer for hydrolase-based biosensors is proposed. In this work, a combination of creatinine deaminase and urease has been chosen as a model system to demonstrate the construction of urea and creatinine biosensors to illustrate the principle. Immobilisation of enzymes was shown to be a crucial step in the development of the biosensors; the use of glycerol and lactitol as stabilisers resulted in a significant improvement, especially in the case of the creatinine, of the operational stability of the biosensors (from few hours to at least 3 days). The developed biosensors exhibited high selectivity towards creatinine and urea. The sensitivity was found to be 85 ± 3.4 mAM(-1)cm(-2) for the creatinine biosensor and 112 ± 3.36 mAM(-1)cm(-2) for the urea biosensor, with apparent Michaelis-Menten constants (KM,app), obtained from the creatinine and urea calibration curves, of 0.163 mM for creatinine deaminase and 0.139 mM for urease, respectively. The biosensors responded linearly over the concentration range 1-125 µM, with a limit of detection of 0.5 µM and a response time of 15s. The performance of the biosensors in a real sample matrix, serum, was evaluated and a good correlation with standard spectrophotometric clinical laboratory techniques was found.

  16. 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.

  17. 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.

  18. Preparation of SiC based Aluminium metal matrix nano composites by high intensity ultrasonic cavitation process and evaluation of mechanical and tribological properties

    NASA Astrophysics Data System (ADS)

    Murthy, N. V.; Prasad Reddy, A.; Selvaraj, N.; Rao, C. S. P.

    2016-09-01

    Request augments on a worldwide scale for the new materials. The metal matrix nano composites can be used in numerous applications of helicopter structural parts, gas turbine exit guide vane's, space shuttle, and other structural applications. The key mailman to ameliorate performance of composite matrix in aluminium alloy metal reinforces nano particles in the matrix of alloy uniformly, which ameliorates composite properties without affecting limit of ductility. The ultrasonic assisted stir casting helped agitation was successfully used to fabricate Al 2219 metal matrix of alloy reinforced with (0.5, 1, 1.5 and 2) wt.% of nano silicon carbide (SiC) particles of different sizes 50nm and 150nm. The micrographs of scanning electron microscopy of nano composite were investigated it reveals that the uniform dispersion of nano particles silicon carbide in aluminium alloy 2219 matrix and with the low porosity. How the specific wear rate was vary with increasing weight percentage of nano particles at constant load and speed as shown in results and discussions. And the mechanical properties showed that the ultimate tensile strength and hardness of metal matrix nano composite AA 2219 / nano SiC of 50nm and 150nm lean to augment with increase weight percentage of silicon carbide content in the matrix alloy.

  19. Magnetization enhancement due to incorporation of non-magnetic nitrogen content in (Co{sub 84}Zr{sub 16})N{sub x} nano-composite films

    SciTech Connect

    Singh, Jitendra Akhtar, Jamil; Shukla, Rishabh; Bagri, Anita; Dhaka, Rajendra S.

    2016-01-15

    We report the magnetic, electronic, and structural properties of nano-composite (Co{sub 84}Zr{sub 16})N{sub x} or CZN films prepared by reactive co-sputter deposition method. As-deposited CZN films have shown enhancement in magnetization (M{sub s}) 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.

  20. 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

  1. 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.

  2. Controllable synthesis and adjustable antineoplastic activity of bovine serum albumin-conjugated PbS/Ag2S core/shell nano-composites.

    PubMed

    Wang, Hua-Jie; Yu, Xue-Hong; Cao, Ying; Zhou, Bei; Wang, Cai-Feng

    2012-08-01

    Series of mono-dispersed bovine serum albumin (BSA)-conjugated PbS/Ag(2)S core/shell nano-composites with different Pb/Ag ratios had been successfully synthesized by an ion-exchange method under the gentle conditions using BSA-conjugated PbS nano-crystals as precursors, which were prepared by a biomimetic method. Fourier transform infrared spectra analysis and transmission electron microscopy (TEM) observation demonstrated that BSA was a key factor to control the morphology and size of final products. Additionally, the real-time TEM observation, X-ray powder diffraction and atomic absorption spectroscopy analysis were applied to monitor the synthesis process. The results indicated that the shell thickness and ratio of Pb to Ag could be controlled by adjusting the ion-exchange time. Both metabolic and morphological methods revealed that the proliferation of rat pheochromocytoma (PC 12) cells could be inhibited by BSA-conjugated PbS/Ag(2)S core/shell nano-composites, and the antineoplastic activity was Pb/Ag ratio-dependent. It might be explained by a Trojan horse-type mechanism. Summarily, the present study would be helpful to find a new core/shell nano-composite with higher and controllable antineoplastic activity due to the synergistic reaction of different metal ions.

  3. High photocatalytic degradation activity of the polyvinyl chloride (PVC)-vitamin C (VC)-TiO2 nano-composite film.

    PubMed

    Yang, Changjun; Gong, Chuqing; Peng, Tianyou; Deng, Kejian; Zan, Ling

    2010-06-15

    A novel photodegradable polyvinyl chloride (PVC)-vitamin C (VC)-TiO(2) nano-composite film was prepared by embedding VC modified nano-TiO(2) photocatalyst into the commercial PVC plastic. The solid-phase photocatalytic degradation behavior of PVC-VC-TiO(2) nano-composite film under UV light irradiation was investigated and compared with those of the PVC-TiO(2) film and the pure PVC film, with the aid of UV-Vis spectroscopy, scanning electron microscopy (SEM), weight loss monitoring, and X-ray diffraction spectra (XRD). The results show that PVC-VC-TiO(2) nano-composite film has a high photocatalytic activity; the photocatalytic degradation rate of it is two times higher than that of PVC-TiO(2) film and fifteen times higher than that of pure PVC film. The optimal mass ratio of VC to TiO(2) is found to be 0.5. The mechanism of enhancing photocatalytic activity is attributed to the formation of a Ti(IV)-VC charge-transfer complex with five-member chelate ring structure and a rapid photogenerated charge separation is thus achieved.

  4. Enhanced adsorption of the cationic dyes in the spherical CuO/meso-silica nano composite and impact of solution chemistry.

    PubMed

    Liang, Zhijie; Zhao, Zhiwei; Sun, Tianyi; Shi, Wenxin; Cui, Fuyi

    2017-01-01

    In this study, the spherical mesoporous silica (meso-silica MCM-41) and that inorganically modified with CuO (CuO/MCM-41 nano composite) were synthesized and characterized. It was demonstrated that CuO were successfully loaded in the synthesized nano composite CuO/MCM-41. Importantly, the loaded CuO had a significant enhancement effect on the adsorption of Crystal violet and Methylene blue. Adsorption kinetic of the tested cationic dyes in the synthesized materials fitted the pseudo-second-order kinetic model and Weber's intra-particle diffusion model well. According to the Langmuir isotherm model, the maximum adsorption capacities (Qmax) of the CuO/MCM-41 towards Crystal violet and Methylene blue increased to 52.9 and 87.8mg/g, while those of the pure MCM-41 were 46.2 and 65.7mg/g, respectively. Due to the surface charge of CuO and the protonation of the dye molecules, the electrostatic forces between the loaded CuO and the organic cationic dyes contributed to the enhancement effect. Additionally, the presented results indicated that the adsorption of the cationic dyes in the CuO/MCM-41 depended on pH and ion strength of the solution but insignificantly on the coexisted humic acid due to the mesoporous character of CuO/MCM-41 nano composite.

  5. 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.

  6. 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

  7. 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

    2015-11-09

    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.

  8. Fabrication of polypyrrole nano-arrays in lysozyme single crystals

    NASA Astrophysics Data System (ADS)

    England, Matt W.; Lambert, Elizabeth M.; Li, Mei; Turyanska, Lyudmila; Patil, Avinash J.; Mann, Stephen

    2012-10-01

    A template-directed method for the synthesis and organization of partially oxidized polypyrrole (PPy) nanoscale arrays within the solvent channels of glutaraldehyde-cross-linked lysozyme single crystals is presented. Macroscopic single crystals of the periodically arranged protein-polymer superstructure are electrically conductive, insoluble in water and organic solvents, and display increased levels of mechanical plasticity compared with native cross-linked lysozyme crystals.A template-directed method for the synthesis and organization of partially oxidized polypyrrole (PPy) nanoscale arrays within the solvent channels of glutaraldehyde-cross-linked lysozyme single crystals is presented. Macroscopic single crystals of the periodically arranged protein-polymer superstructure are electrically conductive, insoluble in water and organic solvents, and display increased levels of mechanical plasticity compared with native cross-linked lysozyme crystals. Electronic supplementary information (ESI) available: Optical microscopy, SEM, TEM images, FTIR spectra and tables, conductivity plot. Experimental methods. See DOI: 10.1039/c2nr32413j

  9. Bulk synthesis of polypyrrole nanofibers by a seeding approach.

    PubMed

    Zhang, Xinyu; Manohar, Sanjeev K

    2004-10-13

    The morphology of doped polypyrrole.Cl powder changes dramatically from granular to nanofibrillar when a very small amount (1-4 mg) of V2O5 nanofibers are added to a chemical oxidative polymerization of pyrrole in aq 1.0 M HCl using (NH4)2S2O8 as the oxidant. Unlike the polyaniline system, a key synthetic requirement in the polypyrrole system is for the seed template to be "active", i.e., to be capable of independently oxidizing the pyrrole monomer. Thin, strongly adherent films can be obtained on inert surfaces such as glass, plastics, etc., directly from the polymerization mixture without any bulk product isolation steps, significantly simplifying the processing of these nanofibers.

  10. Immobilization of tyrosinase in polysiloxane/polypyrrole copolymer matrices.

    PubMed

    Arslan, Ahu; Kiralp, Senem; Toppare, Levent; Yagci, Yusuf

    2005-04-01

    Immobilization of tyrosinase in conducting copolymer matrices of pyrrole functionalized polydimethylsiloxane/polypyrrole (PDMS/PPy) was achieved by electrochemical polymerization. The polysiloxane/polypyrrole/tyrosinase electrode was constructed by the entrapment of enzyme in conducting matrices during electrochemical copolymerization. Maximum reaction rate (V(max)) and Michaelis-Menten constant (K(m)) were investigated for immobilized enzyme. Enzyme electrodes were prepared in two different electrolyte/solvent systems. The effect of supporting electrolytes, p-toluene sulfonic acid and sodium dodecyl sulfate on the enzyme activity and film morphology were determined. Temperature and pH optimization, operational stability and shelf-life of enzyme electrodes were also examined. Phenolic contents of green and black tea were determined by using enzyme electrodes.

  11. A Quartz Microbalance Study of the Electrosynthesis of Polypyrrole

    DTIC Science & Technology

    1988-07-12

    polythiophene. polypyrrole and poly(N-methylpyrrole) have been studied electrochemically using cyclic voltammetry (CV), chronocoulometry... data the theoretical amount of material which should be deposited on the face of the mass sensing crystal can be calculated from a modified version of... data points and has a slope proportional to 2.3 electrons/pyrrole with a V value of 0.9998 for the square of the correlation coefficient (r2). This

  12. Polypyrrole Stability and Coatings for Radar Absorbing Materials

    DTIC Science & Technology

    2004-12-01

    organiques . Dans cet article, on examine la chimie du polypyrrole électro-conducteur et les facteurs relatifs à la préparation de revêtements faits à partir...l’absorbeur. Les absorbeurs faits de matériaux organiques tels que des polymères conducteurs sont légers et présentent des propriétés qu’il est possible de

  13. Band gap modulation in polythiophene and polypyrrole-based systems

    PubMed Central

    Kaloni, Thaneshwor P.; Schreckenbach, Georg; Freund, Michael S.

    2016-01-01

    In this paper, the structural and electronic properties of polythiophene and polyprrrole-based systems have been investigated using first-principles calculations both in periodic and oligomer forms. Of particular interest is the band gap modulation through substitutions and bilayer formation. Specifically, S has been substituted by Se and Te in polythiophene, leading to polyseleophene and polytellurophene, respectively, and N has been substituted by P and As in polypyrrole. The values obtained of the binding energy suggest that all the systems studied can be realized experimentally. Stacking (bilayer formation) of pure polythiophene, polypyrrole and their derivatives leads to linear suppression of the band gap or HOMO-LUMO gap as a function of the stacking. Mixed bilayers, including one formed from polythiophene on top of polypyrrole, have also been considered. Overall, a wide range of band gaps can be achieved through substitutions and stacking. Hybrid (B3LYP) calculations also suggest the same trend in the band gap as PBE calculations. Trends in the binding energy are similar for both periodic and molecular calculations. In addition, Γ-point phonon calculations were performed in order to check the stability of selected systems. PMID:27827393

  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. 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.

  16. Integrated sample pretreatment system for N-linked glycosylation site profiling with combination of hydrophilic interaction chromatography and PNGase F immobilized enzymatic reactor via a strong cation exchange precolumn.

    PubMed

    Qu, Yanyan; Xia, Simin; Yuan, Huiming; Wu, Qi; Li, Man; Zou, Lijuan; Zhang, Lihua; Liang, Zhen; Zhang, Yukui

    2011-10-01

    An integrated sample pretreatment system, composed of a click maltose hydrophilic interaction chromatography (HILIC) column, a strong cation exchange (SCX) precolumn, and a PNGase F immobilized enzymatic reactor (IMER), was established for the simultaneous glycopeptide enrichment, sample buffer exchange, and online deglycosylation, by which the sample pretreatment for glycoproteome could be performed online automatically, beneficial to improve the efficiency and sensitivity of the N-linked glycosylation site identification. With such a system, the deglycosylated glycopeptide from the digests of avidin with the coexistence of 50 times (mass ratio) BSA could be selectively detected, and the detection limit as low as 5 fmol was achieved. Moreover, the sample pretreatment time was significantly shortened to ~1 h. Such a system was further successfully applied for analyzing the digest of the soluble fraction extracted from rat brain. A total of 120 unique glycoprotein groups and 196 N-linked glycosylation sites were identified by nanoreversed phase liquid chromatography-electrospray ionization-tandem mass spectrometry (nanoRPLC-ESI-MS/MS), with the injected digests amount as 6 μg. All these results demonstrate that the integrated system is of great promise for N-linked glycosylation site profiling and could be further online coupled with nanoHPLC-ESI-MS/MS to achieve high-throughput glycoproteome analysis.

  17. 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

    2016-01-05

    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.

  18. Cation exchange-based facile aqueous synthesis of small, stable, and nontoxic near-infrared Ag₂Te/ZnS core/shell quantum dots emitting in the second biological window.

    PubMed

    Chen, Chi; He, Xuewen; Gao, Li; Ma, Nan

    2013-02-01

    Facile aqueous synthesis of near-infrared Ag(2)Te quantum dots (QDs) and Ag(2)Te/ZnS core/shell QDs emitting in the second biological window is reported. The QD synthesis is based on a straightforward cation exchange process between CdTe QDs and Ag(+) ions conducted in aqueous solution. The prepared Ag(2)Te QDs possess near-infrared emission ranging from 900 to 1300 nm and a quantum yield up to 2.1%. A ZnS shell was grown on the Ag(2)Te QD to further enhance the photoluminescence intensity with a quantum yield of 5.6%. These Ag(2)Te/ZnS core/shell QDs possess robust colloidal stability and photostability with minimum photoluminescence fluctuation upon incubation for 72 h in biological buffer or continuous laser excitation for 120 min. Also, These QDs possess small hydrodynamic size (∼7.6 nm) and are non-cytotoxic to human cells, which is ideal for optical bioimaging in the second biological window.

  19. Adsorption of silver ions on polypyrrole embedded electrospun nanofibrous polyethersulfone membranes.

    PubMed

    Wu, Jiunn-Jong; Lee, Hsiu-Wen; You, Jiann-Hwa; Kau, Yi-Chuan; Liu, Shih-Jung

    2014-04-15

    In this study we developed polypyrrole embedded electrospun nanofibrous polyethersulfone nanofibrous membranes for the removal of silver ions. Polypyrrole and polyethersulfone dissolved in N-methyl-2-pyrrolidone (NMP) were electrospun into nanofibrous membranes via an electrospinning process. The morphology of as-spun polypyrrole/polyethersulfone nanofibers was examined by scanning electron microscopy. The average diameter of electrospun nanofibers ranged from 410 nm to 540 nm. The adsorption capability of nanofibrous polypyrrole/polyethersulfone membranes was measured and compared with that of bulk polypyrrole. The influence of various process conditions on adsorption efficiency was also examined. The experimental results suggested that the electrospun nanofibrous membranes exhibited good silver ion uptake capabilities. The metal uptake of nanofibrous membranes increased with the initial metal ion concentrations and the pH value, while decreased with the temperature and the filtering rate of the solutions. Furthermore, the electrospun membrane could be reused after the recovery process.

  20. 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.

  1. 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.

  2. Characterizing reactive oxygen generation and bacterial inactivation by a zerovalent iron-fullerene nano-composite device at neutral pH under UV-A illumination.

    PubMed

    Erdim, Esra; Badireddy, Appala Raju; Wiesner, Mark R

    2015-01-01

    A nano-composite device composed of nano-scale zerovalent iron (ZVI) and C60 fullerene aggregates (ZVI/nC60) was produced via a rapid nucleation method. The device was conceived to deliver reactive oxygen species (ROS) generated by photosensitization and/or electron transfer to targeted contaminants, including waterborne pathogens under neutral pH conditions. Certain variations of the nano-composite were fabricated differing in the amounts of (1) ZVI (0.1mM and 2mM) but not nC60 (2.5mg-C/L), and (2) nC60 (0-25mg-C/L) but not ZVI (0.1mM). The generation of ROS by the ZVI/nC60 nano-composites and ZVI nanoparticles was quantified using organic probe compounds. 0.1mM ZVI/2.5mg-C/L C60 generated 3.74-fold higher O2(-) concentration and also resulted in an additional 2-log inactivation of Pseudomonas aeruginosa when compared to 0.1mM ZVI (3-log inactivation). 2mM ZVI/2.5mg-C/L nC60 showed negligible improvement over 2mM ZVI in terms of O2(-) generation or inactivation. Further, incremental amounts of nC60 in the range of 0-25mg-C/L in 0.1mM ZVI/nC60 led to increased O2(-) concentration, independent of UV-A. This study demonstrates that ZVI/nC60 device delivers (1) enhanced O2(-) with nC60 as a mediator for electron transfer, and (2) (1)O2 (only under UV-A illumination) at neutral pH conditions.

  3. Novel germanium/polypyrrole composite for high power lithium-ion batteries.

    PubMed

    Gao, Xuanwen; Luo, Wenbin; Zhong, Chao; Wexler, David; Chou, Shu-Lei; Liu, Hua-Kun; Shi, Zhicong; Chen, Guohua; Ozawa, Kiyoshi; Wang, Jia-Zhao

    2014-08-29

    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.

  4. Identification of plant and animal glues in museum objects by GC-MS, after catalytic hydrolysis of the proteins by the use of a cation exchanger, with simultaneous separation from the carbohydrates.

    PubMed

    Schneider, U; Kenndler, E

    2001-09-01

    A method is described which enables the group-separation of proteinaceous binding media from vegetable glues (carbohydrates), and simultaneous hydrolysis of the proteins in mixtures of both. The mixtures of the binders are suspended in aqueous-ethanolic solvent with the H+ form of a strong cation exchanger and treated at elevated temperature in sealed vials. The polypeptides are cleaved by H+-catalysed hydrolysis. On abstraction the amino acids are transformed into the ammonium ions by the protons, and the cations are adsorbed by the exchanger resin. The amino acids are removed from solution in this way, thus suppressing interfering reactions with other binders, e.g. humin formation with carbohydrates. Clear and colourless solutions were obtained with all mixtures of vegetable and animal glues. Two fractions can be obtained after separation of the solid resin from the liquid supernatant - the resin fraction with the adsorbed amino acids, and the aqueous-ethanolic solution with the carbohydrates. In each of these fractions the two classes of binder can be identified separately by GC-MS; this avoids the occurrence of unresolved GC peaks and superimposed mass spectra. The method has been used to identify the binder found between fabric layers of a Burgundian liturgical vestment of the Order of the Golden Fleece from the first half of the 15th century, the Cope of the Virgin Mary. With the aid of the GC pattern obtained, and the mass spectra of the main peaks, which were identified as glucopyranose anomers, the binding medium was identified as starch.

  5. Effect of a pharmaceutical cationic exchange resin on the properties of controlled release diphenhydramine hydrochloride matrices using Methocel K4M or Ethocel 7cP as matrix formers.

    PubMed

    Akkaramongkolporn, Prasert; Ngawhirunpat, Tanasait; Nunthanid, Jurairat; Opanasopit, Praneet

    2008-01-01

    This work was aimed at evaluating the effect of a pharmaceutical cationic exchange resin (Amberlite IRP-69) on the properties of controlled release matrices using Methocel K4M (HPMC) or Ethocel 7cP (EC) as matrix formers. Diphenhydramine hydrochloride (DPH), which was cationic and water soluble, was chosen as a model drug. HPMC- and EC-based matrices with varying amounts (0-40%w/w) of resin incorporation were prepared by a direct compression. Matrix properties including diameter, thickness, hardness, friability, surface morphology and drug release were evaluated. The obtained matrices were comparable in diameter and thickness regardless of the amount of resin incorporation. Increasing the incorporated resin decreased the hardness of HPMC- and EC-based matrices, correlating with the degree of rupturing on the matrix surfaces. The friability of HPMC-based matrices increased with increasing the incorporated resin, corresponding to their decreased hardness. In contrast, the EC-based matrices showed no significant change in friability in spite of decreasing hardness. The incorporated resin differently influenced DPH release from HPMC- and EC-based matrices in deionized water. The resin further retarded DPH release from HPMC-based matrices due to the gelling property of HPMC and the ion exchange property of the resin. In contrast, the release from EC-based matrices initially increased because of the disintegrating property of the resin, but thereafter declined due to the complex formation between released drug and dispersed resin via the ion exchange process. The release in ionic solutions was also described. In conclusion, the incorporated resin could alter the release and physical properties of matrices.

  6. Evaluation of bi-functionalized mesoporous silicas as reversed phase/cation-exchange mixed-mode sorbents for multi-residue solid phase extraction of veterinary drug residues in meat samples.

    PubMed

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

    2017-04-01

    A SBA-15 type mesoporous silica was synthesized and bi-functionalized with octadecylsilane (C18) or octylsilane (C8), and sulfonic acid (SO3(-)) groups in order to obtain materials with reversed-phase/strong cation-exchange mixed-mode retention mechanism. The resulting hybrid materials (SBA-15-C18-SO3(-) and SBA-15-C8-SO3(-)) were comprehensively characterized. They showed high surface area, high pore volume and controlled porous size. Elemental analysis of the materials revealed differences in the amount of C18 and C8. SBA-15-C18-SO3(-) contained 0.19mmol/g of C18, while SBA-15-C8-SO3(-) presented 0.54mmol/g of C8. The SO3(-) groups anchored to the silica surface of the pore walls were 0.20 and 0.09mmol/g, respectively. The bi-functionalized materials were evaluated as SPE sorbents for the multi-residue extraction of 26 veterinary drug residues in meat samples using ultra-high-performance liquid chromatography coupled to mass spectrometry detector (UHPLC-MS/MS). Different sorbent amounts (100 and 200mg) and organic solvents were tested to optimize the extraction procedure. Both silicas showed big extraction potential and were successful in the extraction of the target analytes. The mixed-mode retention mechanism was confirmed by comparing both silicas with SBA-15 mesoporous silica mono-functionalized with C18 and C8. Best results were achieved with 200mg of SBA-15-C18-SO3(-) obtaining recoveries higher than 70% for the majority of analytes.

  7. Development and validation of an automated method for the liquid chromatographic determination of sotalol in plasma using dialysis and trace enrichment on a cation-exchange pre-column as on-line sample preparation.

    PubMed

    Chiap, P; Ceccato, A; Miralles Buraglia, B; Boulanger, B; Hubert, P; Crommen, J

    2001-03-01

    A fully automated method for the determination of sotalol in human plasma was developed, involving dialysis through a cellulose acetate membrane, clean-up and enrichment of the dialysate on a strong cation-exchange pre-column and subsequent liquid chromatographic (LC) analysis with UV detection. All sample handling operations were carried out by means of an ASTED system. Before starting dialysis, the trace enrichment column (TEC) was conditioned. The plasma sample, to which the internal standard (atenolol) was automatically added, was then loaded in the donor channel and was kept static while the dialysis liquid, consisting of 0.017 M acetic acid, was passed through the acceptor channel in successive pulses. After each pulse, the dialysate was dispensed onto the TEC. When dialysis was discontinued, the analytes were eluted from the TEC by the LC mobile phase by rotation of a switching valve and transferred to the analytical column packed with octyl silica. The LC mobile phase was a mixture of methanol and pH 7.0 phosphate buffer containing 1-octanesulfonate at a concentration of 7.5 x 10(-4) M (19:81; v/v). The UV detection was performed at 230 nm. The influence of several parameters of the dialysis and trace enrichment processes on analyte recovery and method selectivity was investigated. The method was then validated. The mean absolute recovery for sotalol was about 60%. The limit of quantitation was 25 ng/ml and R.S.D. for repeatability and intermediate precision obtained at a concentration level of 50 ng/ml were 4.3 and 5.8%, respectively.

  8. 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 0.4 mL/min with gradient elution over 3.5 min. 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 0.0251 mg/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.

  9. 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.

  10. 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.

  11. Nano-composite polymer gel electrolytes containing ortho-nitro benzoic acid: role of dielectric constant of solvent and fumed silica

    NASA Astrophysics Data System (ADS)

    Kumar, R.

    2015-03-01

    In this paper, nano-composite polymer gel electrolytes containing polymethylmethacrylate, dimethylacetamide, diethyl carbonate, fumed silica and ortho-nitro benzoic acid have been synthesized. Electrical conductivity, viscosity, pH and thermal behavior of these electrolytes have been studied. The effect of acid, polymer, fumed silica concentration on conductivity, pH and viscosity has been discussed. The effect of dielectric constant of solvent on conductivity behavior of composite polymer gel electrolytes has also been studied. Two maxima in conductivity behavior have been observed with fumed silica concentration for composite polymer gel electrolytes, which have been explained on the basis of double percolation threshold model. Maximum conductivity of 3.20 × 10-4 and 2.46 × 10-6 S/cm at room temperature has been observed for nano-composite polymer gel electrolytes containing 10 wt% polymethylmethacrylate in 1 M solution of o-nitro benzoic acid in dimethylacetamide and diethyl carbonate respectively. The intensity of first maximum observed in conductivity at low concentration of fumed silica has been found to decrease with the decrease in acid concentration for composite polymer gel electrolytes, while the intensity of second maximum at higher fumed silica concentration remains unaffected. The conductivity of composite gels does not show much change in the temperature range of 20-100 °C and also remains constant with time, making them suitable for use as electrolytes in various devices like fuel cells, proton batteries, electrochromic window applications etc.

  12. 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.

  13. Effect of high energy electron beam (10MeV) on specific heat capacity of low-density polyethylene/hydroxyapatite nano-composite.

    PubMed

    Soltani, Z; Ziaie, F; Ghaffari, M; Beigzadeh, A M

    2017-02-01

    In the present work, thermal properties of low density polyethylene (LDPE) and its nano composites are investigated. For this purpose LDPE reinforced with different weight percents of hydroxyapatite (HAP) powder which was synthesized via hydrolysis method are produced. The samples were irradiated with 10MeV electron beam at doses of 75 to 250kGy. Specific heat capacity measurement have been carried out at different temperatures, i.e. 25, 50, 75 and 100°C using modulated temperature differential scanning calorimetry (MTDSC) apparatus and the effect of three parameters include of temperature, irradiation dose and the amount of HAP nano particles as additives on the specific heat capacity of PE/HAP have been investigated precisely. The MTDSC results indicate that the specific heat capacity have decreased by addition of nano sized HAP as reinforcement for LDPE. On the other hand, the effect of radiation dose is reduction in the specific heat capacity in all materials including LDPE and its nano composites. The HAP nano particles along with cross-link junctions due to radiation restrain the movement of the polymer chains in the vicinity of each particle and improve the immobility of polymer chains and consequently lead to reduction in specific heat capacity. Also, the obtained results confirm that the radiation effect on the specific heat capacity is more efficient than the reinforcing effect of nano-sized hydroxyapatite.

  14. The evaluation of prepared microgroove pattern by femtosecond laser on alumina-zirconia nano-composite for endosseous dental implant application.

    PubMed

    Aivazi, Moluk; Hossein Fathi, Mohammad; Nejatidanesh, Farahnaz; Mortazavi, Vajihesadat; HashemiBeni, Batoul; Matinlinna, Jukka Pekka; Savabi, Omid

    2016-12-01

    Ceramic dental materials, especially alumina (20 %vol)-yttrium stabilized tetragonal zirconia poly crystal (A-Y-TZP20), have been considered as alternatives to metals for endosseous dental implant application. For increasing the bone-to-implant contact as well as the speed of bone formation, a new surface modification can be effective. The aim of this study was to design microgroove patterns by femtosecond laser on A-Y-TZP20 nano-composite disks for endosseous dental implant application. The phase composition and the morphology of the A-Y-TZP20 nano-composite samples were characterized using X-ray diffraction and Scanning electron microscopy equipped with energy dispersive X-ray spectroscopy techniques. Statistical analysis was submitted to Kolmogorov-Smirnov test and Student's t test for independent variables, with a 5 % significance level. EDAX analysis revealed a significant decrease in the relative content of contaminants like carbon (p < 0.05) in laser surface-treated group as compared to non surface-treated group. X-ray diffraction did not show any change in the crystalline structure induced by laser processing. It was concluded that the femtosecond laser is a clean and safe method for surface modification of A-Y-TZP20.

  15. Impact ionisation mass spectrometry of polypyrrole-coated pyrrhotite microparticles

    NASA Astrophysics Data System (ADS)

    Hillier, Jon K.; Sternovsky, Zoltan; Armes, Steven P.; Fielding, Lee A.; Postberg, Frank; Bugiel, Sebastian; Drake, Keith; Srama, Ralf; Kearsley, Anton T.; Trieloff, Mario

    2014-07-01

    Cation and anion impact ionization mass spectra of polypyrrole-coated pyrrhotite cosmic dust analogue particles are analysed over a range of cosmically relevant impact speeds. Spectra with mass resolutions of 150-300 were generated by hypervelocity impacts of charged particles, accelerated to up to 37 km s-1 in a Van de Graaff electrostatic accelerator, onto a silver target plate in the Large Area Mass Analyzer (LAMA) spectrometer. Ions clearly indicative of the polypyrrole overlayer are identified at masses of 93, 105, 117, 128 and 141 u. Organic species, predominantly derived from the thin (20 nm) polypyrrole layer on the surface of the particles, dominate the anion spectra even at high (>20 km s-1) impact velocities and contribute significantly to the cation spectra at velocities lower than this. Atomic species from the pyrrhotite core (Fe and S) are visible in all spectra at impact velocities above 6 km s-1 for 56Fe+, 9 km s-1 for 32S+ and 16 km s-1 for 32S- ions. Species from the pyrrhotite core are also frequently visible in cation spectra at impact speeds at which surface ionisation is believed to dominate (<10 km s-1), although the large number of organic peaks complicates the identification of characteristic molecular species. A thin oxidised surface layer on the pyrrhotite particles is indicated by weak spectral features assigned to iron oxides and iron oxy-hydroxides, although the definitive identification of sulfates and hydrated sulfates from the oxidation process was not possible. Silver was confirmed as an excellent choice for the target plate of an impact ionization mass spectrometer, as it provided a unique isotope signature for many target-projectile cluster peaks at masses above 107-109 u. The affinity of Ag towards a dominant organic fragment ion (CN-) derived from fragmentation of the polypyrrole component led to molecular cluster formation. This resulted in an enhanced sensitivity to a particular particle component, which may be of great use

  16. 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.

  17. 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.

  18. 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.

  19. Facile fabrication of AgCl@polypyrrole-chitosan core-shell nanoparticles and polymeric hollow nanospheres.

    PubMed

    Cheng, Daming; Xia, Haibing; Chan, Hardy Sze On

    2004-11-09

    A one-step sequential method for preparing AgCl@polypyrrole-chitosan core-shell nanoparticles and subsequently the formation of polypyrrole-chitosan hollow nanospheres is reported. The formation of the core and the shell is performed in one reaction medium almost simultaneously. Transmission electron microscopy (TEM) images show the presence of core-shell nanoparticles and hollow nanospheres. Ultraviolet-visible (UV-vis) studies reveal that AgCl was formed first followed by polypyrrole. X-ray diffration (XRD) and UV-vis studies show that AgCl was present in the core-shell nanoparticles and could be removed completely from the core.

  20. 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.

  1. 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.

  2. 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.

  3. 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

  4. 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.

  5. The template-assisted synthesis of polypyrrole hollow microspheres with a double-shelled structure.

    PubMed

    Niu, Chunyu; Zou, Bingfang; Wang, Yongqiang; Chen, Lin; Zheng, Haihong; Zhou, Shaomin

    2015-03-25

    Double-shelled polypyrrole hollow microspheres were synthesized via a novel template-assisted concept, using iron oxide hollow microspheres as both the sacrificial template and initiator in acidic solution.

  6. In situ polymerization of highly dispersed polypyrrole on reduced graphite oxide for dopamine detection.

    PubMed

    Qian, Tao; Yu, Chenfei; Wu, Shishan; Shen, Jian

    2013-12-15

    A composite consisting of reduced graphite oxide and highly dispersed polypyrrole nanospheres was synthesized by a straightforward technique, by in situ chemical oxidative polymerization. The novel polypyrrole nanospheres can prevent the aggregation of reduced graphite oxide sheets by electrostatic repulsive interaction, and enhance their electrochemical properties in the nano-molar measurement of dopamine in biological systems with a linear range of 1-8000 nM and a detection limit as low as 0.3 nM.

  7. 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

  8. 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

    NASA Astrophysics Data System (ADS)

    Habibi, Mohammad Hossein; Mardani, Maryam

    2015-02-01

    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.

  9. 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.

  10. 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

  11. Intense white light emission in Tm3+/Er3+/Yb3+ co-doped Y2O3-ZnO nano-composite

    NASA Astrophysics Data System (ADS)

    Yadav, R. S.; Verma, R. K.; Rai, S. B.

    2013-07-01

    The Tm3+/Er3+/Yb3+ co-doped Y2O3-ZnO nano-composite is synthesized using the solution combustion technique. The structural morphology is monitored using x-ray diffraction, transmission electron microscopy and scanning electron microscopy. The Yb3+/Tm3+ co-doped nano-phosphor emits intense blue as well as weak red emissions, while Yb3+/Er3+ co-doped nano-phosphor emits strong green along with red emissions on excitation with 976 nm laser. Joining these together (i.e. Tm3+/Er3+/Yb3+ co-doped phosphor) give very strong white light, which is further verified by CIE coordinates (0.32, 0.36). The addition of ZnO with Y2O3 phosphor gives further enhancement in the intensity of white light. The possible reason for this enhancement is the removal of optical quenching sites.

  12. Organic-inorganic nano-composite films for photonic applications made by multi-beam multi-target pulsed laser deposition with remote control of the plume directions

    NASA Astrophysics Data System (ADS)

    Darwish, Abdalla M.; Moore, Shaelynn; Mohammed, Aziz; Alexander, Deonte'; Bastian, Tyler; Dorlus, Wydglif; Sarkisov, Sergey S.; Patel, Darayas N.; Mele, Paolo; Koplitz, Brent

    2016-09-01

    There has been an explosive interest in the technique of laser assisted deposition of polymer nano-composite films exploiting the matrix assisted pulsed laser evaporation (MAPLE) with regard to the polymer host as can be judged form recent publications.1-4 In MAPLE, a frozen solution of a polymer in a relatively volatile solvent is used as a laser target. The solvent and concentration are selected so that first, the polymer of interest can dissolve to form a dilute, particulate free solution, second, the majority of the laser energy is initially absorbed by the solvent molecules and not by the solute molecules, and third, there is no photochemical reaction between the solvent and the solute. The light-material interaction in MAPLE can be described as a photothermal process. The photon energy absorbed by the solvent is converted to thermal energy that causes the polymer to be heated but the solvent to vaporize. As the surface solvent molecules are evaporated into the gas phase, polymer molecules are exposed at the gas-target matrix interface. The polymer molecules attain sufficient kinetic energy through collective collisions with the evaporating solvent molecules, to be transferred into the gas phase. By careful optimization of the MAPLE deposition conditions (laser wavelength, repetition rate, solvent type, concentration, temperature, and background gas and gas pressure), this process can occur without any significant polymer decomposition. The MAPLE process proceeds layer-by-layer, depleting the target of solvent and polymer in the same concentration as the starting matrix. When a substrate is positioned directly in the path of the plume, a coating starts to form from the evaporated polymer molecules, while the volatile solvent molecules are evacuated by the pump from the deposition chamber. In case of fabrication of polymer nanocomposites, MAPLE targets are usually prepared as nano-colloids of the additives of interest in the initial polymer solutions. Mixing

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. Adsorption of hexavalent chromium onto sisal pulp/polypyrrole composites

    NASA Astrophysics Data System (ADS)

    Tan, Y. Y.; Wei, C.; Gong, Y. Y.; Du, L. L.

    2017-02-01

    Sisal pulp/polypyrrole composites(SP/PPy) utilized for the removal of hexavalent chromium [Cr(VI)] from wastewater, were prepared via in-situ chemical oxidation polymerization approach. The structure and morphology of the SP/PPy were analyzed by polarizing optical microscopy (POM), field-emission scanning electron microscopy (SEM)), Energy-dispersive X-ray spectroscopy (EDS) and X-ray photoelectron spectroscopy (XPS), the results indicated SP could be efficient dispersion of PPy. The hexavalent chromium adsorption results indicate adsorption capacity of the SP/PPy were dependent on the initial pH, with an optimum pH of 2.0. The sorption kinetic data fitted well to the pseudo-second order model and isotherm data fitted well to the Langmuir isotherm model. The maximum adsorption capacity determined from the Langmuir isotherm is 336.70 mg/g at 25° C.

  18. 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.

  19. Electrochemical deposition of conductive and adhesive polypyrrole-dopamine films.

    PubMed

    Kim, Semin; Jang, Lindy K; Park, Hyun S; Lee, Jae Young

    2016-07-27

    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.

  20. Ammonia gas sensor based on electrosynthesized polypyrrole films.

    PubMed

    Carquigny, Stéphanie; Sanchez, Jean-Baptiste; Berger, Franck; Lakard, Boris; Lallemand, Fabrice

    2009-04-15

    In this work, design and fabrication of micro-gas-sensors, polymerization and deposition of poly(pyrrole) thin films as sensitive layer for the micro-gas-sensors by electrochemical processing, and characterization of the polymer films by FTIR, X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM), are reported. The change in conductance of thin polymer layers is used as a sensor signal. The behaviours, including sensitivity, reproducibility and reversibility, to various ammonia gas concentrations ranging from 8 ppm to 1000 ppm are investigated. The influence of the temperature on the electrical response of the sensors is also studied. The experimental results show that these ammonia gas sensors are efficient since they are sensitive to ammonia, reversible and reproducible at room temperature.

  1. 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

  2. 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.

  3. Polypyrrol/chitosan hydrogel hybrid microfiber as sensing artificial muscle

    NASA Astrophysics Data System (ADS)

    Ismail, Yahya A.; Martínez, Jose G.; Al Harrasi, Ahmad S.; Kim, Seon J.; Fernández Otero, Toribio F.

    2011-04-01

    An electrochemical actuator demands that it should act as a sensor of the working conditions for its efficient application in devices. Actuation and sensing characteristics of a biopolymer/conducting polymer hybrid microfiber artificial muscle fabricated through wet spinning of a chitosan solution followed by in situ chemical polymerization with pyrrol employing bis(triflouro methane sulfonyl) imide as dopant and ferric chloride as a catalyst is presented. The polypyrrol/chitosan hybrid microfiber was investigated by FTIR, scanning electron microscopy (SEM), electrical conductivity measurement, cyclic voltammetric and chronopotentiometric methods. The electrochemical measurements related to the sensing abilities were performed as a function of applied current, concentration and temperature keeping two of the variables constant at a given time using NaCl as electrolyte. Cyclic voltammograms confirmed that the electro activity is imparted by polypyrrol (pPy). The fiber showed an electrical conductivity of 3.21x10-1 Scm-1and an average linear electrochemical actuation strain of 0.54%. The chronopotentiometric responses during the oxidation/reduction processes of the microfiber for the different anodic/cathodic currents and the linear fit observed for the consumed electrical energy during the reaction for various applied currents suggested that it can act as a sensor of applied current. The chronopotentiometric responses and the linear fit of consumed electrical energy at different temperatures suggested that the actuator can act as a temperature sensor. Similarly a semi logarithmic dependence of the consumed electrical energy with concentration of the electrolyte during reaction is suggestive of its applicability as a concentration sensor. The demand that an electrochemical actuator to be a sensor of the working conditions, for its efficient application in devices is thus verified in this material.

  4. Understanding the gas sensing properties of polypyrrole coated tin oxide nanofiber mats

    NASA Astrophysics Data System (ADS)

    Bagchi, Sudeshna; Ghanshyam, C.

    2017-03-01

    Tin oxide-polypyrrole composites have been widely studied for their enhanced sensing performance towards ammonia vapours, but further investigations are required for an understanding of the interaction mechanisms with different target analytes. In this work, polypyrrole coated tin oxide fibers have been synthesized using a two-step approach of electrospinning and vapour phase polymerization for the sensing of ammonia, ethanol, methanol, 2-propanol and acetone vapours. The resistance variation in the presence of these vapours of different nature and concentration is investigated for the determination of sensor response. A decrease in resistance occurred on interaction of tin oxide-polypyrrole with ammonia, as opposed to previous reported works. Partial reduction of polypyrrole due to interfacial interaction with tin oxide has been proposed to explain this behavior. High sensitivity of 7.45 is achieved for 1 ppm ammonia concentration. Furthermore, the sensor exhibited high sensitivity and a faster response towards ethanol vapours although methanol has the highest electron donating capability. The catalytic mechanism has been discussed to explain this interesting behavior. The results reveal that interaction between tin oxide and polypyrrole is crucial to control the predominant sensing mechanism.

  5. 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.

  6. 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.

  7. Conducting polypyrrole films as a potential tool for electrochemical treatment of azo dyes in textile wastewaters.

    PubMed

    Haque, Md Mominul; Smith, Warren T; Wong, Danny K Y

    2015-01-01

    In this paper, we demonstrate conducting polypyrrole films as a potential green technology for electrochemical treatment of azo dyes in wastewaters using Acid Red 1 as a model analyte. These films were synthesised by anodically polymerising pyrrole in the presence of Acid Red 1 as a supporting electrolyte. In this way, the anionic Acid Red 1 is electrostatically attracted to the cationic polypyrrole backbone formed to maintain electroneutrality, and is thus entrapped in the film. These Acid Red 1-entrapped polypyrrole films were characterised by electrochemical, microscopic and spectroscopic techniques. Based on a two-level factorial design, the solution pH, Acid Red 1 concentration and polymerisation duration were identified as significant parameters affecting the entrapment efficiency. The entrapment process will potentially aid in decolourising Acid Red 1-containing wastewaters. Similarly, in a cathodic process, electrons are supplied to neutralise the polypyrrole backbone, liberating Acid Red 1 into a solution. In this work, following an entrapment duration of 480 min in 2000 mg L(-1) Acid Red 1, we estimated 21% of the dye was liberated after a reduction period of 240 min. This allows the recovery of Acid Red 1 for recycling purposes. A distinctive advantage of this electrochemical Acid Red 1 treatment, compared to many other techniques, is that no known toxic by-products are generated in the treatment. Therefore, conducting polypyrrole films can potentially be applied as an environmentally friendly treatment method for textile effluents.

  8. Doping Polypyrrole Films with 4-N-Pentylphenylboronic Acid to Enhance Affinity towards Bacteria and Dopamine

    PubMed Central

    Padiolleau, Laurence; Chen, Xi; Jafari, Mohammad Javad; Sheikhzadeh, Elham; Turner, Anthony P. F.; Jager, Edwin W. H.; Beni, Valerio

    2016-01-01

    Here we demonstrate the use of a functional dopant as a fast and simple way to tune the chemical affinity and selectivity of polypyrrole films. More specifically, a boronic-functionalised dopant, 4-N-Pentylphenylboronic Acid (PBA), was used to provide to polypyrrole films with enhanced affinity towards diols. In order to prove the proposed concept, two model systems were explored: (i) the capture and the electrochemical detection of dopamine and (ii) the adhesion of bacteria onto surfaces. The chemisensor, based on overoxidised polypyrrole boronic doped film, was shown to have the ability to capture and retain dopamine, thus improving its detection; furthermore the chemisensor showed better sensitivity in comparison with overoxidised perchlorate doped films. The adhesion of bacteria, Deinococcus proteolyticus, Escherichia coli, Streptococcus pneumoniae and Klebsiella pneumoniae, onto the boric doped polypyrrole film was also tested. The presence of the boronic group in the polypyrrole film was shown to favour the adhesion of sugar-rich bacterial cells when compared with a control film (Dodecyl benzenesulfonate (DBS) doped film) with similar morphological and physical properties. The presented single step synthesis approach is simple and fast, does not require the development and synthesis of functional monomers, and can be easily expanded to the electrochemical, and possibly chemical, fabrication of novel functional surfaces and interfaces with inherent pre-defined sensing and chemical properties. PMID:27875555

  9. Doping Polypyrrole Films with 4-N-Pentylphenylboronic Acid to Enhance Affinity towards Bacteria and Dopamine.

    PubMed

    Golabi, Mohsen; Padiolleau, Laurence; Chen, Xi; Jafari, Mohammad Javad; Sheikhzadeh, Elham; Turner, Anthony P F; Jager, Edwin W H; Beni, Valerio

    2016-01-01

    Here we demonstrate the use of a functional dopant as a fast and simple way to tune the chemical affinity and selectivity of polypyrrole films. More specifically, a boronic-functionalised dopant, 4-N-Pentylphenylboronic Acid (PBA), was used to provide to polypyrrole films with enhanced affinity towards diols. In order to prove the proposed concept, two model systems were explored: (i) the capture and the electrochemical detection of dopamine and (ii) the adhesion of bacteria onto surfaces. The chemisensor, based on overoxidised polypyrrole boronic doped film, was shown to have the ability to capture and retain dopamine, thus improving its detection; furthermore the chemisensor showed better sensitivity in comparison with overoxidised perchlorate doped films. The adhesion of bacteria, Deinococcus proteolyticus, Escherichia coli, Streptococcus pneumoniae and Klebsiella pneumoniae, onto the boric doped polypyrrole film was also tested. The presence of the boronic group in the polypyrrole film was shown to favour the adhesion of sugar-rich bacterial cells when compared with a control film (Dodecyl benzenesulfonate (DBS) doped film) with similar morphological and physical properties. The presented single step synthesis approach is simple and fast, does not require the development and synthesis of functional monomers, and can be easily expanded to the electrochemical, and possibly chemical, fabrication of novel functional surfaces and interfaces with inherent pre-defined sensing and chemical properties.

  10. Antimicrobial activity and cytotoxicity of cotton fabric coated with conducting polymers, polyaniline or polypyrrole, and with deposited silver nanoparticles

    NASA Astrophysics Data System (ADS)

    Maráková, Nela; Humpolíček, Petr; Kašpárková, Věra; Capáková, Zdenka; Martinková, Lenka; Bober, Patrycja; Trchová, Miroslava; Stejskal, Jaroslav

    2017-02-01

    Cotton fabric was coated with conducting polymers, polyaniline or polypyrrole, in situ during the oxidation of respective monomers. Raman and FTIR spectra proved the complete coating of substrates. Polypyrrole content was 19.3 wt.% and that of polyaniline 6.0 wt.%. Silver nanoparticles were deposited from silver nitrate solutions of various concentrations by exploiting the reduction ability of conducting polymers. The content of silver was up to 11 wt.% on polypyrrole and 4 wt.% on polyaniline. The sheet resistivity of fabrics was determined. The conductivity was reduced after deposition of silver. The chemical cleaning reduced the conductivity by less than one order of magnitude for polypyrrole coating, while for polyaniline the decrease was more pronounced. The good antibacterial activity against S. aureus and E. coli and low cytotoxicity of polypyrrole-coated cotton, both with and without deposited silver nanoparticles

  11. Three-dimensional graphene-polypyrrole hybrid electrochemical actuator

    NASA Astrophysics Data System (ADS)

    Liu, Jia; Wang, Zhi; Zhao, Yang; Cheng, Huhu; Hu, Chuangang; Jiang, Lan; Qu, Liangti

    2012-11-01

    The advancement of mechanical actuators benefits from the development of new structural materials with prominent properties. A novel three-dimensional (3D) hydrothermally converted graphene and polypyrrole (G-PPy) hybrid electrochemical actuator is presented, which is prepared via a convenient hydrothermal process, followed by in situ electropolymerization of pyrrole. The 3D pore-interconnected G-PPy pillar exhibits strong actuation responses superior to pure graphene and PPy film. In response to the low potentials of +/-0.8 V, the saturated strain of 3D G-PPy pillar can reach a record of 2.5%, which is more than 10 times higher than that of carbon nanotube film and about 3 times that of unitary graphene film under an applied potential of +/-1.2 V. Also, the 3D G-PPy actuator exhibits high actuation durability with high operating load as demonstrated by an 11 day continuous measurement. Finally, a proof-of-concept application of 3D G-PPy as smart filler for on/off switch is also demonstrated, which indicates the great potential of the 3D G-PPy structure developed in this study for advanced actuator systems.The advancement of mechanical actuators benefits from the development of new structural materials with prominent properties. A novel three-dimensional (3D) hydrothermally converted graphene and polypyrrole (G-PPy) hybrid electrochemical actuator is presented, which is prepared via a convenient hydrothermal process, followed by in situ electropolymerization of pyrrole. The 3D pore-interconnected G-PPy pillar exhibits strong actuation responses superior to pure graphene and PPy film. In response to the low potentials of +/-0.8 V, the saturated strain of 3D G-PPy pillar can reach a record of 2.5%, which is more than 10 times higher than that of carbon nanotube film and about 3 times that of unitary graphene film under an applied potential of +/-1.2 V. Also, the 3D G-PPy actuator exhibits high actuation durability with high operating load as demonstrated by an 11 day

  12. 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.

  13. Electrical characterization and hydrogen peroxide sensing properties of gold/Nafion:polypyrrole/MWCNTs electrochemical devices.

    PubMed

    Scandurra, Graziella; Arena, Antonella; Ciofi, Carmine; Saitta, Gaetano

    2013-03-19

    Electrochemical devices using as substrates copier grade transparency sheets are developed by using ion conducting Nafion:polypyrrole mixtures, deposited between gold bottom electrodes and upper electrodes based on Multi Walled Carbon Nanotubes (MWCNTs). The electrical properties of the Nafion:polypyrrole blends and of the gold/Nafion:polypyrrole/MWCNTs devices are investigated under dry conditions and in deionized water by means of frequency dependent impedance measurements and time domain electrical characterization. According to current-voltage measurements carried out in deionized water, the steady state current forms cycles characterized by redox peaks, the intensity and position of which reversibly change in response to H2O2, with a lower detection limit in the micromolar range. The sensitivity that is obtained is comparable with that of other electrochemical sensors that however, unlike our devices, require supporting electrolytes.

  14. 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.

  15. Improved Electromagnetic Shielding Performance of Lightweight Compression Molded Polypyrrole/Ferrite Composite Sheets

    NASA Astrophysics Data System (ADS)

    Varshney, Swati; Dhawan, S. K.

    2017-01-01

    An attempt has been made to design lightweight polypyrrole/carbon fibers and polypyrrole/carbon fibers/ferrofluid (Fe3O4 particles) composite sheets using novolac resin via compression molding for electromagnetic shielding applications. The optimized formulation has been achieved to get an excellent combination of thermal, mechanical, and electrical properties of the composite sheet. Structural and morphological studies were carried out by x-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy. Polypyrrole/carbon fibers composite sheets shows maximum flexural strength and a flexural modulus of 62.4 ± 1 MPa and 0.60 ± 0.02 GPa, respectively, with total shielding effectiveness of 22.8 dB in the Ku-band (12.4-18 GHz) but when ferrofluid is added to the polypyrrole/carbon fibers composite system, flexural strength increases to 92.3 ± 1 MPa and the same trend has been observed for flexural modulus with a value of 0.65 ± 0.04 GPa. This multiphase lightweight polypyrrole composite sheet having 34 vol.% of carbon fibers and 4 vol.% of Fe3O4 nanoparticles offers total shielding effectiveness of 31.9 dB (>99.99% attenuation) in the Ku-band (12.4-18 GHz) frequency range with a thickness of ˜1.25 mm. This is accredited to high dielectric losses and magnetic losses in conducting composite sheets. The observed results suggest that lightweight compression molded polypyrrole composite sheets could be a potential commercial alternative for electromagnetic shielding applications.

  16. Kinetic model and thermodynamic study of Acid Red 1 entrapment at electropolymerised polypyrrole films.

    PubMed

    Haque, Md Mominul; Wong, Danny K Y

    2015-11-01

    This work is focussed on the determination of a kinetic model and the thermodynamic study of the electrochemical entrapment of the model azo dye, Acid Red 1, at conducting polypyrrole films, which is proposed as a potential green technology for treatment of azo dyes in industrial effluents. The entrapment kinetic data were found to follow a pseudosecond order model involving an intra-particle diffusion. However, the equilibrium data obtained for Acid Red 1 entrapment at polypyrrole did not obey any common surface adsorption models such as the Langmuir, Freundlich, Temkin and Dubinin-Radushkevich isotherms. Accordingly, the entrapment process may lead to an enhanced quantity of dye embedded in a polypyrrole film, making it a more effective and efficient technology than those involving only adsorption. Similarly, dye leakage from polypyrrole film surface to a sample matrix will be easily prevented. For this treatment process, a negative ΔG° range between -1.46±0.78 and -2.94±0.24 kJ mol(-1) at the corresponding temperature range of 298-318 K, and a ΔH° of 20.5±2.5 kJ mol(-1) indicate a spontaneous and endothermic entrapment process. Also, a positive ΔS° (73.6±8.2 J mol(-1) K(-1)) reveals increased randomness of the interface and an affinity of Acid Red 1 towards polypyrrole films. A low activation energy (7.67±0.80 kJ mol(-1)) confirms a physical process for Acid Red 1 entrapment at polypyrrole films.

  17. Improved Electromagnetic Shielding Performance of Lightweight Compression Molded Polypyrrole/Ferrite Composite Sheets

    NASA Astrophysics Data System (ADS)

    Varshney, Swati; Dhawan, S. K.

    2017-03-01

    An attempt has been made to design lightweight polypyrrole/carbon fibers and polypyrrole/carbon fibers/ferrofluid (Fe3O4 particles) composite sheets using novolac resin via compression molding for electromagnetic shielding applications. The optimized formulation has been achieved to get an excellent combination of thermal, mechanical, and electrical properties of the composite sheet. Structural and morphological studies were carried out by x-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy. Polypyrrole/carbon fibers composite sheets shows maximum flexural strength and a flexural modulus of 62.4 ± 1 MPa and 0.60 ± 0.02 GPa, respectively, with total shielding effectiveness of 22.8 dB in the Ku-band (12.4-18 GHz) but when ferrofluid is added to the polypyrrole/carbon fibers composite system, flexural strength increases to 92.3 ± 1 MPa and the same trend has been observed for flexural modulus with a value of 0.65 ± 0.04 GPa. This multiphase lightweight polypyrrole composite sheet having 34 vol.% of carbon fibers and 4 vol.% of Fe3O4 nanoparticles offers total shielding effectiveness of 31.9 dB (>99.99% attenuation) in the Ku-band (12.4-18 GHz) frequency range with a thickness of ˜1.25 mm. This is accredited to high dielectric losses and magnetic losses in conducting composite sheets. The observed results suggest that lightweight compression molded polypyrrole composite sheets could be a potential commercial alternative for electromagnetic shielding applications.

  18. CONDENSED MATTER: ELECTRONIC STRUCTURE, ELECTRICAL, MAGNETIC, AND OPTICAL PROPERTIES: Enhanced nonlinear optical absorption of Au/SiO2 nano-composite thin films

    NASA Astrophysics Data System (ADS)

    Zhao, Cui-Hua; Zhang, Bo-Ping; Shang, Peng-Peng

    2009-12-01

    Nano metal-particle dispersed glasses are the attractive candidates for nonlinear optical material applications. Au/SiO2 nano-composite thin films with 3 vol% to 65 vol% Au are prepared by inductively coupled plasma sputtering. Au particles as perfect spheres with diameters between 10 nm and 30 nm are uniformly dispersed in the SiO2 matrix. Optical absorption peaks due to the surface plasmon resonance of Au particles are observed. The absorption property is enhanced with the increase of Au content, showing a maximum value in the films with 37 vol% Au. The absorption curves of the Au/SiO2 thin films with 3 vol% to 37 vol% Au accord well with the theoretical optical absorption spectra obtained from Mie resonance theory. Increasing Au content over 37 vol% results in the partial connection of Au particles, whereby the intensity of the absorption peak is weakened and ultimately replaced by the optical absorption of the bulk. The band gap decreases with Au content increasing from 3 vol% to 37 vol% but increases as Au content further increases.

  19. 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.

  20. 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.

  1. 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.

  2. 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.

  3. Up-conversion luminescence in Yb(3+)-Er(3+)/Tm(3+) co-doped Al2O3-TiO2 nano-composites.

    PubMed

    Mokoena, Teboho Patrick; Linganiso, Ella Cebisa; Kumar, Vinod; Swart, Hendrik C; Cho, So-Hye; Ntwaeaborwa, Odireleng Martin

    2017-06-15

    The sol gel method was used to prepare rare-earths (Yb(3+)-Er(3+) and Yb(3+)-Tm(3+)) co-doped Al2O3-TiO2 nano-composite powder phosphors and their up-conversion luminescence properties were investigated. Mixed oxides of titania (TiO2) rutile phase and an early stage crystallization of alumina (Al2O3) phase were confirmed from the X-ray diffraction data with the average crystallite size of ∼36nm. The rutile phase TiO2 was further confirmed by selected area diffraction analysis of the composites. Microscopy analysis showed interesting rod-like morphologies with rough surfaces indicating that a spherulitic growth process took place during the crystal growth. Photoluminescence characterization of the phosphors was carried out under near infra-red excitation at 980nm and the prominent emission bands were observed in the visible region at 523, 548 and 658nm for the Yb(3+)-Er(3+) co-doped systems. Emission in bands extending from the visible to near infra-red regions were observed at 480, 650, 693 and 800nm for the Yb(3+)-Tm(3+) co-doped systems. These upconverted emissions and energy transfer mechanisms taking place are discussed in detail.

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. Adaptive Tempering Monte Carlo Study of Dense Polypyrrole Systems

    NASA Astrophysics Data System (ADS)

    Dai, Yafei; Blaisten-Barojas, Estela

    2009-03-01

    A modified rigid-ion polarizable model potential of polypyrrole is developed with parameters fitted on multiple points of the electronic energy surface of pyrrole oligomers (n-Py) of different sizes calculated with a hybrid density functional approach [1]. Using this potential, systems containing 192 chains (4-Py) and 64 chains (12-Py) were structurally optimized with the Adaptive Tempering Monte Carlo algorithm [2]. Energetics and structure of these systems were studied as a function of density. Both systems have characteristics of a liquid for densities in the range 0.66 -- 1.09 g/cm^3 at T=300 K. The oligomer radius of gyration is insensitive to density changes. However, an orientational order parameter shows a sharp increase as a function of density indicating a tendency of the chains to stack forming regions of aligned chains for the denser systems. [1] Y. Dai, E. Blaisten-Barojas, J. Chem. Phys. 129, 164903(2008); [2] X. Dong, E. Blaisten-Barojas, J. Comp. & Theo. Nanoscience 3, 118 (2006).

  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. Polypyrrole-Coated Electrospun PLGA Nanofibers for Neural Tissue Applications

    PubMed Central

    Lee, Jae Young; Bashur, Chris A.; Goldstein, Aaron S.; Schmidt, Christine E.

    2009-01-01

    Electrospinning is a promising approach to create nanofiber structures that are capable of supporting adhesion and guiding extension of neurons for nerve regeneration. Concurrently, electrical stimulation of neurons in the absence of topographical features also has been shown to guide axonal extension. Therefore, the goal of this study was to form electrically conductive nanofiber structures and to examine the combined effect of nanofiber structures and electrical stimulation. Conductive meshes were produced by growing polypyrrole (PPy) on random and aligned electrospun poly(lactic-co-glycolic acid) (PLGA) nanofibers, as confirmed by scanning electron micrographs and X-ray photon spectroscopy. PPy-PLGA electrospun meshes supported the growth and differentiation of rat pheochromocytoma 12 (PC12) cells and hippocampal neurons comparable to non-coated PLGA control meshes, suggesting that PPy-PLGA may be suitable as conductive nanofibers for neuronal tissue scaffolds. Electrical stimulation studies showed that PC12 cells, stimulated with a potential of 10 mV/cm on PPy-PLGA scaffolds, exhibited 40–50% longer neurites and 40–90% more neurite formation compared to unstimulated cells on the same scaffolds. In addition, stimulation of the cells on aligned PPy-PLGA fibers resulted in longer neurites and more neurite-bearing cells than stimulation on random PPy-PLGA fibers, suggesting a combined effect of electrical stimulation and topographical guidance and the potential use of these scaffolds for neural tissue applications. PMID:19501901

  11. Training effect and fatigue in polypyrrole-based artificial muscles.

    PubMed

    Kaneto, Keiichi; Suematsu, Hirotaka; Yamato, Kentaro

    2008-09-01

    Artificial muscles based on an electrochemomechanical strain (ECMS) in conducting polymers, namely polypyrrole (PPy) film, have been studied from viewpoints of training, fatigue and aging by repeat cycles under tensile loads. ECMS was approximately 2% in a saline solution, resulting from both insertion and exclusion of Na(+) with solvated water molecules as well in the film. Transient responses of ECMS and current induced by voltage stimuli were measured under tensile stresses up to 5 MPa to see the training effect, fatigue and aging of the film. At higher stresses the film showed larger creeping, which resulted from realignment or conformation change, slipping and breaking of polymer chains. After the experience of large stresses, the training effect in ECMS was appreciably observed as an increase of the strain. Without stress the conductivity of the film was stable (no fatigue) upon an electrochemical cycle; however, under high tensile stresses the conductivity decreased remarkably (fatigue and aging). It is to be noted that straightened polymer chains can be easily oxidized and degraded due to lower pi-electron energy. The conversion efficiency from electrical to mechanical energy in this system was found to be less than 0.03%.

  12. 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.

  13. Bile salt incorporated polypyrrole thin film for ethanol sensing.

    PubMed

    Sharma, Partha P D; Sarkar, D

    2015-04-01

    Polypyrrole (PPy)-bile salt composite was used for sensing ethanol vapor. PPy was synthesized by interface polymerization for subsequent fabrication of thin film of its composite with bile salt, by in-situ co-dispersion method and then exposed to ethanol vapour. Sensing was visualized through changes in morphological, structural and optical characterizations. The ethanol exposed film showed larger agglomeration as revealed in its surface morphology on scanning electron microscope (SEM) and greater crystallinity as seen through X-Ray diffraction (XRD). Fourier transform infra red (FTIR) and nuclear magnetic resonance spectroscopy (NMR) of the ethanol incorporated film also gave signature of the presence of bile salt and alcohol. Alcohol incorporation pattern resulted in increase in electrical conductance from 7.08539 x 10(-5) mA/V to 8.0356 x 10(-5) mA/V, as determined from current voltage characterizations. Average molecular weight (M(n)) obtained from gel permeation chromatography changed from 6160 to 10300 on ethanol intake. Photoluminescence (PL) intensity was quenched and the PL peak shifted from 430 to 409 on ethanol exposure. Changes in morphological, structural, optical and electrical properties of the composite on ethanol exposure showed its prospective application for sensing ethanol.

  14. 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

  15. 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.

  16. Polymer Films on Electrodes. 13. Incorporation of Catalysts into Electronically Conductive Polymers: Iron Phthalocyanine in Polypyrrole.

    DTIC Science & Technology

    1983-04-26

    POLYPYRROLE. Randy A. Bull, Fu-Ren Fan and A. J. Bard Prepared for Publication in the Journal of Electrochemical Society DTIC i The University of Texas...NUMBER 7. AUIMOR(,) N. CONTRACT OR GRANT NUMBER(s) Randy A. Bull, Fu-Ren Fan, Allen J. Bard• ... "N000I 4-78-C-0592 S. PERFORMING ORGANIZATION NAME AND...PHTHALOCYANINE IN POLYPYRROLE. Randy A. Bull, Fu-Ren Fan and A. J. Bard Department of Chemistry, University of Texas at Austin Austin, Texas 78722

  17. Electrochemical synthesis of polypyrrole-Al2O3 composite coating on 316 stainless steel for corrosion protection

    NASA Astrophysics Data System (ADS)

    Yan, Qun; Li, Chuanxian; Huang, Tingting; Yang, Fei

    2017-03-01

    Polypyrrole (PPy)-Al2O3 composite coating was electrochemically deposited on 316 stainless steel (316 SS) by cyclic voltammetry technique. Scanning electron microscopy (SEM) and Fourier transform infrared spectroscopy (FT-IR) were employed to understand the morphology and composition of the PPy-Al2O3 coated SS. The corrosion protection ability of the PPy-Al2O3 coating was studied using open circuit potential (Eocp)-time measurements, polarization curves, and electrochemical impedance spectroscopy (EIS) after the electrodes had been immersed in a 3.5 wt% NaCl solution as the corrosive media. The results showed that PPy-Al2O3 composite coatings have a homogeneous and smooth surface without detectable cracks. Anodic polarization analysis revealed that the hybrid films provided an exceptional barrier and corrosion protection in comparison with PPy coating. The EIS studies indicated that the charge transfer resistance increases with the presence of PPy-Al2O3. PPy-Al2O3 composite coating provides better corrosion protection and can be considered as a coating material to protect 316SS. With increase in Al2O3/Py mole ratio, PPy-Al2O3 coatings tend to exhibit a better corrosion resistance ability.

  18. Cell patterning via linker-free protein functionalization of an organic conducting polymer (polypyrrole) electrode.

    PubMed

    Bax, Daniel V; Tipa, Roxana S; Kondyurin, Alexey; Higgins, Michael J; Tsoutas, Kostadinos; Gelmi, Amy; Wallace, Gordon G; McKenzie, David R; Weiss, Anthony S; Bilek, Marcela M M

    2012-07-01

    The interaction of proteins and cells with polymers is critical to their use in scientific and medical applications. In this study, plasma immersion ion implantation (PIII) was used to modify the surface of the conducting polymer, polypyrrole, which possesses electrical properties. PIII treatment enabled persistent, covalent binding of the cell adhesive protein, tropoelastin, without employing chemical linking molecules. In contrast tropoelastin was readily eluted from the untreated surface. Through this differential persistence of binding, surface bound tropoelastin supported cell adhesion and spreading on the PIII treated but not the untreated polypyrrole surface. The application of a steel shadow mask during PIII treatment allowed for spatial definition of tropoelastin exclusively to PIII treated regions. The general applicability of this approach to other extracellular matrix proteins was illustrated using collagen I, which displayed similar results to tropoelastin but required extended washing conditions. This approach allowed fine patterning of cell adhesion and spreading to tropoelastin and collagen, specifically on PIII treated polypyrrole regions. We therefore present a methodology to alter the functionality of polypyrrole surfaces, generating surfaces that can spatially control cellular interactions through protein functionalization with the potential for electrical stimulation.

  19. One pot synthesis of polypyrrole silver nanocomposite on cotton fabrics for multifunctional property.

    PubMed

    Firoz Babu, K; Dhandapani, P; Maruthamuthu, S; Anbu Kulandainathan, M

    2012-11-06

    Polymer-silver nanocomposites modified cotton fabrics were prepared by in situ chemical oxidative polymerization using pyrrole and silver nitrate. In a redox reaction between pyrrole and silver nitrate, silver ions oxidize the pyrrole monomer and get reduced. This reduced silver as nanoparticles deposited on/into the polypyrrole/cotton matrix layer and the interaction between silver and polypyrrole was by adsorption or electrostatic interaction. The structure and composite formation on cotton fiber was investigated using SEM, FT-IR, XPS and XRD. The results showed that a strong interaction existing between silver nanoparticles with polypyrrole/cotton matrix. FT-IR studies clearly indicated that the interaction between polypyrrole (-N-H) and cellulose (>C-OH) was by hydrogen bonding. It is observed that the conductivity of the composite coated fabrics has been increased by the incorporation of silver nanoparticles. In the synthesized composites, silver content plays an important role in the conductivity and antimicrobial activity rate of the fabrics against gram positive Staphylococcus aureus and gram negative Escherichia coli bacteria.

  20. Photopolymerization of 3D conductive polypyrrole structures via digital light processing

    NASA Astrophysics Data System (ADS)

    Price, Aaron D.

    2016-04-01

    The intrinsically conductive polymer polypyrrole is conventionally synthesized as monolithic films that exhibit significant actuation strains when subjected to an applied electric potential. Though numerous linear and bending actuators based on polypyrrole films have been investigated, the limitations inherent to planar film geometries inhibit the realization of more complex behaviours. Hence, three-dimensional polypyrrole structures are sought to greatly expand the potential applications for conductive polymer actuators. This research aims to develop a novel additive manufacturing method for the fabrication of three-dimensional structures of conductive polypyrrole. In this investigation, radiation-curing techniques are employed by means of digital light processing (DLP) technology. DLP is an additive manufacturing technique where programmed light patterns emitted from a dedicated source are used to selectively cure a specially formulated polymer resin. Successive curing operations lead to a layered 3D structure into which fine features may be incorporated. Energy dispersive spectroscopy (EDS) is subsequently employed to examine the unique microstructural features of the resultant 3D printed polymer morphology in order to elucidate the nature of the conductivity. These polymer microstructures are highly desirable since actuation response times are highly dependent on ion transport distances, and hence the ability to fabricate fine features offers a potential mechanism to improve actuator performance.