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Sample records for hydrated silica gel

  1. Phase equilibria and thermodynamic modeling of ethane and propane hydrates in porous silica gels.

    Science.gov (United States)

    Seo, Yongwon; Lee, Seungmin; Cha, Inuk; Lee, Ju Dong; Lee, Huen

    2009-04-23

    In the present study, we examined the active role of porous silica gels when used as natural gas storage and transportation media. We adopted the dispersed water in silica gel pores to substantially enhance active surface for contacting and encaging gas molecules. We measured the three-phase hydrate (H)-water-rich liquid (L(W))-vapor (V) equilibria of C(2)H(6) and C(3)H(8) hydrates in 6.0, 15.0, 30.0, and 100.0 nm silica gel pores to investigate the effect of geometrical constraints on gas hydrate phase equilibria. At specified temperatures, the hydrate stability region is shifted to a higher pressure region depending on pore size when compared with those of bulk hydrates. Through application of the Gibbs-Thomson relationship to the experimental data, we determined the values for the C(2)H(6) hydrate-water and C(3)H(8) hydrate-water interfacial tensions to be 39 +/- 2 and 45 +/- 1 mJ/m(2), respectively. By using these values, the calculation values were in good agreement with the experimental ones. The overall results given in this study could also be quite useful in various fields, such as exploitation of natural gas hydrate in marine sediments and sequestration of carbon dioxide into the deep ocean.

  2. The dependence of phase change enthalpy on the pore structure and interfacial groups in hydrated salts/silica composites via sol-gel.

    Science.gov (United States)

    Wu, Yuping; Wang, Tao

    2015-06-15

    It was found that the procedures for incorporating hydrated salts into silica, including mixing with sol in an instant (S1 procedure), mixing with sol via drop by drop (S2 procedure) and mixing until the sol forming the gel (S3 procedure), had pronounced effects on the phase change enthalpy of hydrated salts/silica composite via sol-gel process. The discrepancy of phase change enthalpies of the composites with the same content of hydrated salts can be as high as 40 kJ/kg. To unveil the mechanism behind, the pore structure of silica matrix and interfacial functional groups were investigated extensively. It was revealed that different incorporation procedures resulted in distinct pore structure of silica matrix and different intensities of interfacial Si-OH groups. The S3 procedure was beneficial to induce the silica matrix with bigger pore size and fewer Si-OH groups. Consequently, the phase change enthalpy of the hydrated salts/silica composite prepared by this procedure was the highest because of its lower size confinement effects and weaker adsorption by Si-OH groups. This study will provide insight into the preparation of shape-stabilized phase change materials for thermal energy storage applications. Copyright © 2015 Elsevier Inc. All rights reserved.

  3. Silica reinforced triblock copolymer gels

    DEFF Research Database (Denmark)

    Theunissen, E.; Overbergh, N.; Reynaers, H.

    2004-01-01

    The effect of silica and polymer coated silica particles as reinforcing agents on the structural and mechanical properties of polystyrene-poly(ethylene/butylene)-polystyrene (PS-PEB-PS) triblock gel has been investigated. Different types of chemically modified silica have been compared in order...... a viscoclastic rubber to a plastic fluid and from a plastic fluid to a viscoelastic liquid are shifted to more elevated temperatures when silica is added to the triblock copolymer gel. (C) 2004 Elsevier Ltd. All rights reserved....

  4. [Effect of water on silica gel adsorption of blood plasma components].

    Science.gov (United States)

    Gall', L N; Malakhova, M Ia; Melenevskaia, E Iu; Podosenova, N G; Sharonova, L V

    2011-01-01

    In this work, the study of properties of silica gel as an adsorbent for plasmasorption has been performed. Investigations have been realized of the effect of silica gel preliminary treatment conditions and a period of plasma with silica gel contact on plasmasorption characteristics of human blood plasma components, such as protein, triglycerides, cholesterol (high-density and low-density one). The results obtained can be used for variation of silica gel adsorption properties, in situ at the adsorbent preparation process. For explanation of the experimental concentration and kinetic (temporal) characteristics of plasmasorption, the model of silica gel grains charging at the hydration was used.

  5. Metal-silica sol-gel materials

    Science.gov (United States)

    Stiegman, Albert E. (Inventor)

    2002-01-01

    The present invention relates to a single phase metal-silica sol-gel glass formed by the co-condensation of a transition metal with silicon atoms where the metal atoms are uniformly distributed within the sol-gel glass as individual metal centers. Any transition metal may be used in the sol-gel glasses. The present invention also relates to sensor materials where the sensor material is formed using the single phase metal-silica sol-gel glasses. The sensor materials may be in the form of a thin film or may be attached to an optical fiber. The present invention also relates to a method of sensing chemicals using the chemical sensors by monitoring the chromatic change of the metal-silica sol-gel glass when the chemical binds to the sensor. The present invention also relates to oxidation catalysts where a metal-silica sol-gel glass catalyzes the reaction. The present invention also relates to a method of performing oxidation reactions using the metal-silica sol-gel glasses. The present invention also relates to organopolymer metal-silica sol-gel composites where the pores of the metal-silica sol-gel glasses are filled with an organic polymer polymerized by the sol-gel glass.

  6. Consolidation of Inorganic Precipitated Silica Gel

    Directory of Open Access Journals (Sweden)

    Matthias Kind

    2011-08-01

    Full Text Available Colloidal gels are possible intermediates in the generation of highly porous particle systems. In the production process the gels are fragmented after their formation. These gel fragments compact to particles whose application-technological properties are determined by their size and porosity. In the case of precipitated silica gels, this consolidation process depends on temperature and pH, among other parameters. It is shown that these dependencies can be characterized by oedometer measurements. Originally, the oedometer test (one-dimensional compression test stemmed from soil mechanics. It has proven to be an interesting novel examination method for gels. Quantitative data of the time-dependent shrinkage of gel samples can be obtained. The consolidation of the gels shows a characteristic dependence on the above parameters.

  7. Effect of Some Admixtures on the Hydration of Silica Fume and Hydrated Lime

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    The effects of sodium salt of naphthalene formaldehyde sulfonic acid and stearic acid on the hydration of silica fume and Ca(0H)2 have been investigated. The hydration was carried out at 60℃ and W/S ratio of 4 for various time intervals namely, 1, 3, 7 and 28 days and in the presence of 0.2% and 5% superplasticizer and stearic acid. The results of the hydration kinetics show that both admixtures accelerate the hydration reaction of silica fume and calcium hydroxide during the first 7 days. Whereas, after 28 days hydration there is no significant effect. Generally, most of free calcium hydroxide seems to be consumed after 28 days. In addition, the phase composition as well as the microstructure of the formed hydrates was examined by using X-ray diffraction analysis (XRD) and scanning electron microscopy (SEM) respectively.

  8. Soluble polymers in sol-gel silica

    Science.gov (United States)

    Beaudry, Christopher Laurent

    In the last few years, the inherent versatility of sol-gel processing has led to a significant research effort on inorganic/organic materials. One method of incorporating an organic phase into sol-gel silica is dissolving an organic polymer in a tetraethylorthosilicate (TEOS) solution, followed by in situ polymerization of silica in the presence of organic polymer. The first part of the study involved the development of a two-step (acid-base) synthesis procedure to allow systematic control of acidity in TEOS solutions. With this procedure, it was possible to increase the pH of the TEOS solution while correlating the acidity and properties. The properties were the gelation time, syneresis rate, drying behavior, and xerogel pore structure, as determined by nitrogen sorption. Furthermore, controlling the acidity was shown to control the silica xerogel pore structure. In the second part of the study, the two-step procedure was used to synthesize silica/poly(ethylene glycol) (PEG), and silica/poly(vinyl acetate) (PVAc) composite materials. The content of organic polymer and the molecular weight were varied. The gelation time, the syneresis rate, the drying behavior, and the pore structure were determined for compositions with 10% PEG (M.W. 2,000), 5, 10, and 15% PEG (M.W. 3,400), and 10 and 25% PVAc (M.W. 83,000). Other compositions and molecular weights of PEG lead to sedimentation. In the PEG compositions, the tendency to phase separate was correlated with the effects of the processing variables on the segregation strength and polymerization rate. The PVAc compositions did not show any visible phase separation during processing, giving the composite xerogels an appearance similar to pure silica. The property differences between gels with PEG and gels with PVAc show the relative strength of the interactions with silica. Both polymers exhibit hydrogen bonding between the phases. In the case of PEG, hydrogen bonding between the ether oxygens of the polymer and silanol

  9. Silica gel stimulates the hydrolysis of lecithin by phospholipase A

    NARCIS (Netherlands)

    Goerke, J.; Gier, J. de; Bonsen, P.P.M.

    1971-01-01

    1. 1. Silica gel stimulates the hydrolysis of aqueous lecithin suspensions by phospholipase A. The activation is slightly greater than that caused by ether and takes place equally well in bulk suspensions of silica gel or on thin-layer Chromatographic plates prepared with silica. 2. 2. The hydrolys

  10. Effect of heat on the adsorption properties of silica gel

    OpenAIRE

    Christy, Alfred A.

    2012-01-01

    Adsorption properties of silica gel have been attributed to the surface hydroxyl groups of silica gel. Some hydroxyl groups are free standing and called free silanol groups. Some are hydrogen bonded to neighbouring silanol groups. Christy has shown that a high silanol number and a balanced concentration proportionality between these two different types of hydroxyl groups is necessary for effective adsorption of water molecules. Thermal treatment of silica gel samples alters the proportions...

  11. Silica surfaces lubrication by hydrated cations adsorption from electrolyte solutions.

    Science.gov (United States)

    Donose, Bogdan C; Vakarelski, Ivan U; Higashitani, Ko

    2005-03-01

    Adsorption of hydrated cations on hydrophilic surfaces has been related to a variety of phenomena associated with the short-range interaction forces and mechanisms of the adhesive contact between the surfaces. Here we have investigated the effect of the adsorption of cations on the lateral interaction. Using lateral force microscopy (LFM), we have measured the friction force between a silica particle and silica wafer in pure water and in electrolyte solutions of LiCl, NaCl, and CsCl salts. A significant lubrication effect was demonstrated for solutions of high electrolyte concentrations. It was found that the adsorbed layers of smaller and more hydrated cations have a higher lubrication capacity than the layers of larger and less hydrated cations. Additionally, we have demonstrated a characteristic dependence of the friction force on the sliding velocity of surfaces. A mechanism for the observed phenomena based on the microstructures of the adsorbed layers is proposed.

  12. Influence of amorphous silica on the hydration in ultra-high performance concrete

    Energy Technology Data Exchange (ETDEWEB)

    Oertel, Tina, E-mail: tina.oertel@isc.fraunhofer.de [Fraunhofer–Institute for Silicate Research ISC, Neunerplatz 2, 97082 Würzburg (Germany); Inorganic Chemistry I, Universität Bayreuth, Universitätsstr. 30, 95440 Bayreuth (Germany); Helbig, Uta, E-mail: uta.helbig@th-nuernberg.de [Crystallography and X-ray Methods, Technische Hochschule Nürnberg Georg Simon Ohm, Wassertorstraße 10, 90489 Nürnberg (Germany); Hutter, Frank [Fraunhofer–Institute for Silicate Research ISC, Neunerplatz 2, 97082 Würzburg (Germany); Kletti, Holger [Building Materials, Bauhaus–Universität Weimar, Coudraystr. 11, 99423 Weimar (Germany); Sextl, Gerhard [Fraunhofer–Institute for Silicate Research ISC, Neunerplatz 2, 97082 Würzburg (Germany); Chemical Technology of Advanced Materials, Julius Maximilian Universität, Röntgenring 11, 97070 Würzburg (Germany)

    2014-04-01

    Amorphous silica particles (silica) are used in ultra-high performance concretes to densify the microstructure and accelerate the clinker hydration. It is still unclear whether silica predominantly increases the surface for the nucleation of C–S–H phases or dissolves and reacts pozzolanically. Furthermore, varying types of silica may have different and time dependent effects on the clinker hydration. The effects of different silica types were compared in this study by calorimetric analysis, scanning and transmission electron microscopy, in situ X-ray diffraction and compressive strength measurements. The silica component was silica fume, pyrogenic silica or silica synthesized by a wet-chemical route (Stoeber particles). Water-to-cement ratios were 0.23. Differences are observed between the silica for short reaction times (up to 3 days). Results indicate that silica fume and pyrogenic silica accelerate alite hydration by increasing the surface for nucleation of C–S–H phases whereas Stoeber particles show no accelerating effect.

  13. Hierarchically Structured Monolithic ZSM-5 through Macroporous Silica Gel Zeolitization

    Institute of Scientific and Technical Information of China (English)

    Lei Qian; Zhao Tianbo; Li Fengyan; Zong Baoning; Tong Yangchuan

    2006-01-01

    The hierarchically structured ZSM-5 monolith was prepared through transforming the skeletons of the macroporous silica gel into ZSM-5 by the steam-assisted conversion method. The morphology and monolithic shapes of macroporous silica gel were well preserved. The hierarchically structured ZSM-5 monolith exhibited the hierarchical porosity, with mesopores and macropores existing inside the macroporous silica gel, and micropores formed by the ZSM-5. The products have been characterized properly by using the XRD, SEM and N2 adsorption-desorption methods.

  14. Molecular modeling of the dissociation of methane hydrate in contact with a silica surface.

    Science.gov (United States)

    Bagherzadeh, S Alireza; Englezos, Peter; Alavi, Saman; Ripmeester, John A

    2012-03-15

    We use constant energy, constant volume (NVE) molecular dynamics simulations to study the dissociation of the fully occupied structure I methane hydrate in a confined geometry between two hydroxylated silica surfaces between 36 and 41 Å apart, at initial temperatures of 283, 293, and 303 K. Simulations of the two-phase hydrate/water system are performed in the presence of silica, with and without a 3 Å thick buffering water layer between the hydrate phase and silica surfaces. Faster decomposition is observed in the presence of silica, where the hydrate phase is prone to decomposition from four surfaces, as compared to only two sides in the case of the hydrate/water simulations. The existence of the water layer between the hydrate phase and the silica surface stabilizes the hydrate phase relative to the case where the hydrate is in direct contact with silica. Hydrates bound between the silica surfaces dissociate layer-by-layer in a shrinking core manner with a curved decomposition front which extends over a 5-8 Å thickness. Labeling water molecules shows that there is exchange of water molecules between the surrounding liquid and intact cages in the methane hydrate phase. In all cases, decomposition of the methane hydrate phase led to the formation of methane nanobubbles in the liquid water phase.

  15. Steady-state leaching of tritiated water from silica gel

    DEFF Research Database (Denmark)

    Das, H.A.; Hou, Xiaolin

    2009-01-01

    Aqueous leaching of tritium from silica gel, loaded by absorption of water vapor, makes part of reactor de-commissioning. It is found to follow the formulation of steady-state diffusion.......Aqueous leaching of tritium from silica gel, loaded by absorption of water vapor, makes part of reactor de-commissioning. It is found to follow the formulation of steady-state diffusion....

  16. Steady-state leaching of tritiated water from silica gel

    DEFF Research Database (Denmark)

    Das, H.A.; Hou, Xiaolin

    2009-01-01

    Aqueous leaching of tritium from silica gel, loaded by absorption of water vapor, makes part of reactor de-commissioning. It is found to follow the formulation of steady-state diffusion.......Aqueous leaching of tritium from silica gel, loaded by absorption of water vapor, makes part of reactor de-commissioning. It is found to follow the formulation of steady-state diffusion....

  17. Methane Hydrate Formation and Dissociation in the Presence of Silica Sand and Bentonite Clay

    Directory of Open Access Journals (Sweden)

    Kumar Saw V.

    2015-11-01

    Full Text Available The formation and dissociation of methane hydrates in a porous media containing silica sand of different sizes and bentonite clay were studied in the presence of synthetic seawater with 3.55 wt% salinity. The phase equilibrium of methane hydrate under different experimental conditions was investigated. The effects of the particle size of silica sand as well as a mixture of bentonite clay and silica sand on methane hydrate formation and its dissociation were studied. The kinetics of hydrate formation was studied under different subcooling conditions to observe its effects on the induction time of hydrate formation. The amount of methane gas encapsulated in hydrate was computed using a real gas equation. The Clausius-Clapeyron equation is used to estimate the enthalpy of hydrate dissociation with measured phase equilibrium data.

  18. Hybrid silica-PVA nanofibers via sol-gel electrospinning.

    Science.gov (United States)

    Pirzada, Tahira; Arvidson, Sara A; Saquing, Carl D; Shah, S Sakhawat; Khan, Saad A

    2012-04-03

    We report on the synthesis of poly(vinyl alcohol) (PVA)-silica hybrid nanofibers via sol-gel electrospinning. Silica is synthesized through acid catalysis of a silica precursor (tetraethyl orthosilicate (TEOS) in ethanol-water), and fibers are obtained by electrospinning a mixture of the silica precursor solution and aqueous PVA. A systematic investigation on how the amount of TEOS, the silica-PVA ratio, the aging time of the silica precursor mixture, and the solution rheology influence the fiber morphology is undertaken and reveals a composition window in which defect-free hybrid nanofibers with diameters as small as 150 nm are obtained. When soaked overnight in water, the hybrid fibers remain intact, essentially maintaining their morphology, even though PVA is soluble in water. We believe that mixing of the silica precursor and PVA in solution initiates the participation of the silica precursor in cross-linking of PVA so that its -OH group becomes unavailable for hydrogen bonding with water. FTIR analysis of the hybrids confirms the disappearance of the -OH peak typically shown by PVA, while formation of a bond between PVA and silica is indicated by the Si-O-C peak in the spectra of all the hybrids. The ability to form cross-linked nanofibers of PVA using thermally stable and relatively inert silica could broaden the scope of use of these materials in various technologies.

  19. Sol-Gel Synthesis of Non-Silica Monolithic Materials

    Directory of Open Access Journals (Sweden)

    Bartłomiej Gaweł

    2010-04-01

    Full Text Available Monolithic materials have become very popular because of various applications, especially within chromatography and catalysis. Large surface areas and multimodal porosities are great advantages for these applications. New sol-gel preparation methods utilizing phase separation or nanocasting have opened the possibility for preparing materials of other oxides than silica. In this review, we present different synthesis methods for inorganic, non-silica monolithic materials. Some examples of application of the materials are also included.

  20. New silica clathrate minerals that are isostructural with natural gas hydrates.

    Science.gov (United States)

    Momma, Koichi; Ikeda, Takuji; Nishikubo, Katsumi; Takahashi, Naoki; Honma, Chibune; Takada, Masayuki; Furukawa, Yoshihiro; Nagase, Toshiro; Kudoh, Yasuhiro

    2011-02-15

    Silica clathrate compounds (clathrasils) and clathrate hydrates are structurally analogous because both materials have framework structures with cage-like voids occupied by guest species. The following three structural types of clathrate hydrates are recognized in nature: cubic structure I (sI); cubic structure II (sII); and hexagonal structure H (sH). In contrast, only one naturally occurring silica clathrate mineral, melanophlogite (sI-type framework), has been found to date. Here, we report the discovery of two new silica clathrate minerals that are isostructural with sII and sH hydrates and contain hydrocarbon gases. Geological and mineralogical observations show that these silica clathrate minerals are traces of low-temperature hydrothermal systems at convergent plate margins, which are the sources of thermogenic natural gas hydrates. Given the widespread occurrence of submarine hydrocarbon seeps, silica clathrate minerals are likely to be found in a wide range of marine sediments.

  1. Time and frequency dependent rheology of reactive silica gels.

    Science.gov (United States)

    Wang, Miao; Winter, H Henning; Auernhammer, Günter K

    2014-01-01

    In a mixture of sodium silicate and low concentrated sulfuric acid, nano-sized silica particles grow and may aggregate to a system spanning gel network. We studied the influence of the finite solubility of silica at high pH on the mechanical properties of the gel with classical and piezo-rheometers. Direct preparation of the gel sample in the rheometer cell avoided any pre-shear of the gel structure during the filling of the rheometer. The storage modulus of the gel grew logarithmically with time with two distinct growth laws. The system passes the gel point very quickly but still shows relaxation at low frequency, typically below 6 rad/s. We attribute this as a sign of structural rearrangements due to the finite solubility of silica at high pH. The reaction equilibrium between bond formation and dissolution maintains a relatively large bond dissolution rate, which leads to a finite life time of the bonds and behavior similar to physical gels. This interpretation is also compatible with the logarithmic time dependence of the storage modulus. The frequency dependence was more pronounced for lower water concentrations, higher temperatures and shorter reaction times. With two relaxation models (the modified Cole-Cole model and the empirical Baumgaertel-Schausberger-Winter model) we deduced characteristic times from the experimental data. Both models approximately described the data and resulted in similar relaxation times.

  2. Heat and mass transfer during silica gel-moisture interactions

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Jin; Besant, Robert W. [Department of Mechanical Engineering, University of Saskatchewan, 57 Campus Drive, Saskatoon, SK, Canada S7N 5A9 (Canada)

    2005-11-01

    An initially dry granular silica gel bed is subject to a sudden uniform air flow at a selected temperature and humidity. The coupled non-equilibrium heat transfer and moisture transfer were investigated experimentally and numerically. This study provides a fundamental view of heat and mass transfer process within the granular particle pores. It was found that only a small fraction of internal surface area of silica gel is exposed to water vapour during the test and this occurs very slowly with a time delay that must be accounted for in the model. This modified model gives transient response results that agree with the experimental data within the uncertainty bounds. (author)

  3. The Influence of Microgravity on Silica Sol-Gel Formation

    Science.gov (United States)

    Sibille, L.; Smith, D. D.; Cronise, R.; Hunt, A. J.; Wolfe, D. B.; Snow, L. A.; Oldenberg, S.; Halas, N.; Rose, M. Franklin (Technical Monitor)

    2000-01-01

    We discuss space-flight experiments involving the growth of silica particles and gels. The effect of microgravity on the growth of silica particles via the sol-gel route is profound. In four different recipes spanning a large range of the parameter space that typically produces silica nanoparticles in unit-gravity, low-density gel structures were instead formed in microgravity. The particles that did form were generally smaller and more polydisperse than those grown on the ground. These observations suggest that microgravity reduces the particle growth rate, allowing unincorporated species to form aggregates and ultimately gel. Hence microgravity favors the formation of more rarefied structures, providing a bias towards diffusion-limited cluster-cluster aggregation. These results further suggest that in unit gravity, fluid flows and sedimentation can significantly perturb sol-gel substructures prior to gelation and these deleterious perturbations may be "frozen" into the resulting microstructure. Hence, sol-gel pores may be expected to be smaller, more uniform, and less rough when formed in microgravity.

  4. Moisture Transport in Silica Gel Packed Beds: II. Experimental Study

    Energy Technology Data Exchange (ETDEWEB)

    Pesaran, A. A.; Mills, A. F.

    1986-08-01

    Experiments have been performed to obtain the transient response of a thin adiabatic packed bed of silica gel after a step change in inlet air conditions, comparisons are made with predictions using a solid-side resistance model and a pseudo-gas-side controlled model and better agreement obtained with the former model.

  5. A silica gel based method for extracting insect surface hydrocarbons.

    Science.gov (United States)

    Choe, Dong-Hwan; Ramírez, Santiago R; Tsutsui, Neil D

    2012-02-01

    Here, we describe a novel method for the extraction of insect cuticular hydrocarbons using silica gel, herein referred to as "silica-rubbing". This method permits the selective sampling of external hydrocarbons from insect cuticle surfaces for subsequent analysis using gas chromatography-mass spectrometry (GC-MS). The cuticular hydrocarbons are first adsorbed to silica gel particles by rubbing the cuticle of insect specimens with the materials, and then are subsequently eluted using organic solvents. We compared the cuticular hydrocarbon profiles that resulted from extractions using silica-rubbing and solvent-soaking methods in four ant and one bee species: Linepithema humile, Azteca instabilis, Camponotus floridanus, Pogonomyrmex barbatus (Hymenoptera: Formicidae), and Euglossa dilemma (Hymenoptera: Apidae). We also compared the hydrocarbon profiles of Euglossa dilemma obtained via silica-rubbing and solid phase microextraction (SPME). Comparison of hydrocarbon profiles obtained by different extraction methods indicates that silica rubbing selectively extracts the hydrocarbons that are present on the surface of the cuticular wax layer, without extracting hydrocarbons from internal glands and tissues. Due to its surface specificity, efficiency, and low cost, this new method may be useful for studying the biology of insect cuticular hydrocarbons.

  6. Tough ceramic coatings: Carbon nanotube reinforced silica sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Lopez, A.J., E-mail: antoniojulio.lopez@urjc.es [Dept. de Ciencia e Ingenieria de Materiales, ESCET, Universidad Rey Juan Carlos, C/Tulipan s/n, Mostoles 28933, Madrid (Spain); Rico, A.; Rodriguez, J.; Rams, J. [Dept. de Ciencia e Ingenieria de Materiales, ESCET, Universidad Rey Juan Carlos, C/Tulipan s/n, Mostoles 28933, Madrid (Spain)

    2010-08-15

    Silica coatings reinforced with carbon nanotubes were produced via sol-gel route using two mixing techniques of the sol-gel precursors, mechanical and ultrasonic mixing, and dip-coating as deposition process on magnesium alloy substrates. Effective incorporation and distribution of 0.1 wt.% of carbon nanotubes in the amorphous silica matrix of the coatings were achieved using both techniques. Fabrication procedure determines the morphological aspects of the coating. Only mechanical mixing process produced coatings dense and free of defects. Nanoindentation technique was used to examine the influence of the fabrication process in the mechanical features of the final coatings, i.e. indentation fracture toughness, Young's modulus and hardness. A maximum toughening effect of about 24% was achieved in silica coatings reinforced with carbon nanotubes produced by the mechanical mixing route. Scanning electron microscopy investigation revealed that the toughening of these reinforced coatings was mainly due to bridging effect of the reinforcement.

  7. Methane Hydrate Formation and Dissociation in the Presence of Silica Sand and Bentonite Clay

    National Research Council Canada - National Science Library

    Kumar Saw, V; Udayabhanu, G; Mandal, A; Laik, S

    2015-01-01

      The formation and dissociation of methane hydrates in a porous media containing silica sand of different sizes and bentonite clay were studied in the presence of synthetic seawater with 3.55 wt% salinity...

  8. The increase in pH during aging of porous sol-gel silica spheres

    NARCIS (Netherlands)

    Titulaer, M.K.; Kegel, W.K.; Jansen, J.B.H.; Geus, John W.

    1994-01-01

    The increase in pH in the hydrothermal fluid is studied after hydrothermal aging of porous silica gel spheres of 1–3 mm diameter. The porous silica spheres are formed by the sol-gel process from a supersaturated silica solution. The increase of the pH of the hydrothermal solution affects the silica

  9. Analyzing the adsorption of blood plasma components by means of fullerene-containing silica gels and NMR spectroscopy in solids

    Science.gov (United States)

    Melenevskaya, E. Yu.; Mokeev, M. V.; Nasonova, K. V.; Podosenova, N. G.; Sharonova, L. V.; Gribanov, A. V.

    2012-10-01

    The results from studying the adsorption of blood plasma components (e.g., protein, triglycerides, cholesterol, and lipoproteins of low and high density) using silica gels modified with fullerene molecules (in the form of C60 or the hydroxylated form of C60(OH) x ) and subjected to hydration (or, alternatively, dehydration) are presented. The conditions for preparing adsorbents that allow us to control the adsorption capacity of silica gel and the selectivity of adsorption toward the components of blood plasma, are revealed. The nature and strength of the interactions of the introduced components (fullerene molecules and water) with functional groups on the silica surface are studied by means of solid state NMR spectroscopy (NMR-SS). Conclusions regarding the nature of the centers that control adsorption are drawn on the basis of NMR-SS spectra in combination with direct measurements of adsorption. The interaction of the oxygen of the hydroxyl group of silica gel with fullerene, leading to the formation of electron-donor complexes of C60-H, C60-OH, or C60-OSi type, is demonstrated by the observed changes in the NMR-SS spectra of silica gels in the presence of fullerene.

  10. Microporous silica gels from alkylsilicate-water two phase hydrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Chu, L.; Tejedor-Tejedor, M.I.; Anderson, M.A. [Univ. of Wisconsin, Madison, WI (United States). Water Chemistry Program

    1994-12-31

    Microporous silica gels have been synthesized through a nano-particulate sol-gel route. These gels have uniformly distributed and extremely small pores(< 15 {angstrom} in diameter). Hydrolysis and condensation reactions leading to these gels were carried out in an alkyl silicate-water (ammonia) two phase system. These reactions took place at the alkyl silicate droplet-water interfacial boundary. No alcohol was added. A clear, stable and uniformly distributed colloidal silica suspension having an average particle size less than 6 nm was prepared by this method. Fast hydrolysis, slow condensation and low solubility all contribute to a high supersaturation level and result in the formation of small particles. This process is consistent with classic nucleation theory. When the particles are produced under acidic rather than under basic reaction conditions, smaller particles are formed due to the slower condensation rate and lower solubility of these silica particles in acidic conditions. At the same pH, alkylsilicates having smaller alkyl groups react faster with water leading to smaller primary particles. Homogeneous nucleation conditions are achieved when the water/alkylsilicate ratio is high.

  11. Preparation and characterization of carbosilane denddmer-bonded silica gel and its use in LC

    Institute of Scientific and Technical Information of China (English)

    Chen Guowen; Zhao Shigui; Feng Shengyu

    2006-01-01

    Divergently synthesized carbosilane dendrimers generations 1(G1) and 2 (G2) with allyl end groups were bonded onto silica gel.Reactions between the dendrimers and acid-processed silica gel took place,with toluene reflux and organic base as catalyst.Chemically bonded silica gel was characterized by transmission electron microscopy (TEM),infrared (IR),and other methods.The chemically modified silica gels were packed into high-pressure liquid chromatography (HPLC) column and their separation characters were evaluated.G2-bonded silica gel was effective in separating homologous compounds of alcohol, alkyl-substituted benzene,N-substituted benzene,metacrylic acid ester and phthalate.

  12. INVESTIGATION OF THE INTERACTIONS BETWEEN WATER AND MODIFIED SILICA GEL BY IGC AND TPD

    Institute of Scientific and Technical Information of China (English)

    LI Xin; LI Zhong; XIA Qibin; XI Hongxia

    2006-01-01

    In this work, the thermodynamic parameters for the adsorption of water vapor on untreated silica gel and silica gel treated with hygroscopic salts and silane coupling agent were determined by Inverse Gas Chromatography (IGC) in the infinite dilution region. The desorption activation energies of the water vapor on virgin and modified silica gels were estimated by using the Temperature Programmed Desorption (TPD) technique. The interactions between the water and the virgin and modified silica gels were discussed. Results showed that the thermodynamic parameters and desorption activation energy of water vapour on the silica gels increase with decreasing pore size and increasing the surface hydrophilic properties. The desorption activation energy of virgin and modified silica gels was found to increase with increasing the thermodynamic parameters. The larger the adsorption parameters and the desorption activation energy were, the interactions between water and virgin and modified silica gels were.

  13. Preparation of silica by sol-gel method using formamide

    Directory of Open Access Journals (Sweden)

    R.F.S. Lenza

    2001-07-01

    Full Text Available In this work we obtained microporous and mesoporous silica gels by sol-gel processing. Tetraethylortosilicate (TEOS was used as precursor. Nitric acid and hydrofluoric acid were used as catalysts. In order to study the affect of formamide as drying additive, we used a molar ratio alkoxide/formamide of 1/1. The performance of formamide in obtaining crack-free gels was evaluated through monolithicity measurements. The structural evolution occurring in the interconnected network of the gels during thermal treatment was monitored by Fourier transform infrared spectroscopy (FTIR, shrinkage and density measurements and nitrogen gas sorption. We noted that in the presence of formamide, the Si-O-Si bonds are stronger and belong to a more cross-linked structure. The samples obtained in the presence of formamide have larger pore volume and its pore structure is in the range of mesoporosity. The samples obtained without additive are microporous. Formamide allowed the preparation of crack-free silica gels stabilized at high temperatures.

  14. Dynamical Behaviour of H2O in Silica Gel

    Institute of Scientific and Technical Information of China (English)

    王燕; 董顺乐

    2002-01-01

    The vibrational spectra of silica gel with low concentrations of water, 3%0 and 10%, were studied by inelastic neutron scattering at 5 K. The experimental spectrum for 3% water in silica gelshows dramatic changes compared to the spectra for the other known ice phases in the energy transfer region of 2 - 140 meV. Its intermolecular librational band is shifted to lower energy by about 20meV (or by a factor of 1.43) compared to ice Ih, and shows a similar librational band with liquid at 290K. A significant excess of low-frequency vibration modes (< 7 meV)over normal ice Ih and a very wide acoustic peak (4 - 15 meV) were observed. Experimental data indicate that little H2O (3%) in silica gelexhibits a strong softening of hydrogen bonds compared to bulk normal ice and all the other known ice phases.

  15. A Gas Chromatographic Analysis of Light Hydrocarbons on a Column Packed with Modified Silica Gel

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    A one-meter long column packed with silica gel is used to separate light hydrocarbons. The silica gel has been modified with several kinds of gas chromatography stationary phases. Among these, PEG 2000 shows fairly good effect when using 80-100 meshes silica gel for the separation of mixture of methane, ethane, ethylene, acetylene, propane, propylene and n-, i-butane. The different behavior of silica gel between batch to batch is also found. When silica gel is coated with a small amount of Al2O3 prepared with sol-gel method, better resolution has been observed on a 2-meter column compared with the non-modified silica gel.

  16. Hydration and microstructure of Portland cement partially substituted with ultrafine silica

    Directory of Open Access Journals (Sweden)

    Escalante, J. I.

    2009-12-01

    Full Text Available Geothermal waste, a by-product of steam power plants that use geothermal underground resources, was studied as a possible replacement for Portland cement. This waste consists primarily in amorphous nanometric silica with traces of sodium and potassium chlorides. The replacement ratios studied were 0, 10 and 20% in cements cured at 20 and 60 ºC. X-ray diffraction analysis showed that clinker phase hydration took place earlier in the presence of the geothermal waste. Scanning electron microscopy, in turn, revealed a reduction in porosity and intense calcium hydroxide consumption as a result of the pozzolanic reaction. The pastes containing 20% waste, however, an intense cracking was observed due to the formation of alkali silica reaction gel and ettringite. Cracking was more prominent at 60 ºC but was not observed in either the neat cement or the blend with 10 % waste. The presence of these detrimental phases was attributed to the formation of Friedel’s salt in the initial hydration stages, induced by the chlorides in the geothermal material.Se investigaron pastas de cemento Portland sustituido con un desecho geotérmico, subproducto de la generación de electricidad en plantas que emplean recursos geotérmicos. El desecho está compuesto principalmente de sílice amorfa de tamaño nanométrico, con cloruros de sodio y potasio. Se investigaron cementos con niveles de substitución de 0, 10 y 20%, curados a 20 y 60 °C. En presencia del desecho geotérmico, se observó por Difracción de rayos X cuantitativa que la hidratación de las fases del clínker se aceleró; además mediante microscopía electrónica de barrido se encontró una disminución en la porosidad y un intenso consumo de hidróxido de calcio por la reacción puzolánica. Sin embargo, para pastas con 20% de desecho geotérmico, se observó agrietamiento con la presencia de gel de reacción álcali sílice y ettringita; fue más acentuado a 60 °C y no se observó para pastas de

  17. Spherulitic crystallization of holmium tartrates in silica gels

    Energy Technology Data Exchange (ETDEWEB)

    Want, Basharat [University of Kashmir, Department of Physics, Srinagar (India)

    2011-09-15

    Spherulites of holmium tartrate trihydrate and holmium nitro-tartrate monohydrate have been grown in silica gel medium by making holmium nitrate to react with tartaric acid at high supersaturations. The mechanism of spherulitic growth of holmium tartrates is discussed. The spherulitic crystallization is shown to be due to heterogeneous nucleation. In the early stages of growth an amorphous spherical mass gets nucleated inside the gel. Crystal fibers diverge radially from the surface of the spherical mass giving rise to a spherical polycrystalline holmium tartrate. Thermal stability of the two types of spherulites grown in the silica gel shows that the holmium tartrate trihydrate is more stable than holmium nitro-tartrate monohydrate. The surface morphology and internal structure of the spherulites of holmium tartrates have been studied by using scanning electron microscopy. The results on growth kinetics are given by studying the variation of radius of spherulites as a function of time. A non-linear time-size relations under several conditions of growth have been observed, which suggests a non-uniform solute concentration at the crystal surface. (orig.)

  18. Iron Oxide Silica Derived from Sol-Gel Synthesis

    Directory of Open Access Journals (Sweden)

    João Carlos Diniz da Costa

    2011-02-01

    Full Text Available In this work we investigate the effect of iron oxide embedded in silica matrices as a function of Fe/Si molar ratio and sol pH. To achieve homogeneous dispersion of iron oxide particles, iron nitrate nonahydrate was dissolved in hydrogen peroxide and was mixed with tetraethyl orthosilicate and ethanol in a sol-gel synthesis method. Increasing the calcination temperature led to a reduction in surface area, although the average pore radius remained almost constant at about 10 Å, independent of the Fe/Si molar ratio or sol pH. Hence, the densification of the matrix was accompanied by similar reduction in pore volume. However, calcination at 700 °C resulted in samples with similar surface area though the iron oxide content increased from 5% to 50% Fe/Si molar ratio. As metal oxide particles have lower surface area than polymeric silica structures, these results strongly suggest that the iron oxides opposed the silica structure collapse. The effect of sol pH was found to be less significant than the Fe/Si molar ratio in the formation of molecular sieve structures derived from iron oxide silica.

  19. Silica doped with lanthanum sol-gel thin films for corrosion protection

    Energy Technology Data Exchange (ETDEWEB)

    Abuin, M. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Serrano, A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); Llopis, J. [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain); Garcia, M.A. [Glass and Ceramic Institute, CSIC, C. Kelsen 5, 28049 Madrid (Spain); IMDEA Nanoscience, Fco. Tomas y Valiente 7, 28049 Madrid (Spain); Carmona, N., E-mail: n.carmona@fis.ucm.es [Department of Materials Physics, Complutense University at Madrid, Avda. Complutense sn, 28004 Madrid (Spain)

    2012-06-01

    We present here anticorrosive silica coatings doped with lanthanum ions for the protection of metallic surfaces as an alternative to chromate (VI)-based conversion coatings. The coatings were synthesized by the sol-gel method starting from silicon alkoxides and two different lanthanum precursors: La (III) acetate hydrate and La (III) isopropoxide. Artificial corrosion tests in acid and alkaline media showed their effectiveness for the corrosion protection of AA2024 aluminum alloy sheets for coating prepared with both precursors. The X-ray absorption Near Edge Structure and X-ray Absorption Fine Structure analysis of the coatings confirmed the key role of lanthanum in the structural properties of the coating determining its anticorrosive properties. - Highlights: Black-Right-Pointing-Pointer Silica sol-gel films doped with lanthanum ions were synthesized. Black-Right-Pointing-Pointer Films from lanthanum-acetate and La-alkoxide were prepared for comparison purposes. Black-Right-Pointing-Pointer La-acetate is an affordable chemical reactive preferred for the industry. Black-Right-Pointing-Pointer Films properties were explored by scanning electron microscopy and X-Ray absorption spectroscopy. Black-Right-Pointing-Pointer An alternative to anticorrosive pre-treatments for metallic surfaces is suggested.

  20. All-silica nanofluidic devices for DNA-analysis fabricated by imprint of sol-gel silica with silicon stamp

    DEFF Research Database (Denmark)

    Mikkelsen, Morten Bo Lindholm; Letailleur, Alban A; Søndergård, Elin

    2011-01-01

    We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination of the imprin......We present a simple and cheap method for fabrication of silica nanofluidic devices for single-molecule studies. By imprinting sol-gel materials with a multi-level stamp comprising micro- and nanofeatures, channels of different depth are produced in a single process step. Calcination...... of the imprinted hybrid sol-gel material produces purely inorganic silica, which has very low autofluorescence and can be fusion bonded to a glass lid. Compared to top-down processing of fused silica or silicon substrates, imprint of sol-gel silica enables fabrication of high-quality nanofluidic devices without...

  1. Formulation of mefenamic acid loaded transfersomal gel by thin film hydration technique and hand shaking method

    Directory of Open Access Journals (Sweden)

    Krishna Sailaja

    2017-04-01

    Full Text Available Objective(s: The aim of present study is to formulate mefenamic acid transdermal gel based on vesicular drug delivery approaches.Materials and Methods: For the preparation of mefenamic acid transdermal gel, transfersomes were selected as colloidal carriers. Transfersomes were prepared by hand shaking and thin film hydration techniques. The obtained transfersomes were characterized for vesicular diameter, zeta potential, drug content, entrapment efficiency and in vitro diffusion studies.Results: Among Different formulations of transfersomes, T10(prepared by thin film hydration and containing soya lecithin: span60 ratio 1:2 was considered as the best formulation because of its mean vesicular diameter of 369 nm, zeta potential of -14 mV, drug content of 99.6%, entrapment efficiency of 84.4%, and sustained drug release of 93.3% after 12 h.T10 formulation was incorporated into gel. Comparative study was made among plain gel, and transfersomal gel. Among these two gels, transfersomal gel considered as best because of its highest drug content (91%, spreadability (43.5 g.cm/sec, pH (6.9 and sustained drug release profile for 12 h.Conclusion: By comparing  hand shaking and thin film hydration techniques, it was found thin film hydration technique produced better results and transfersomal gel was indicated better results than plain gel.

  2. Adsorption Kinetics at Silica Gel/Ionic Liquid Solution Interface

    Directory of Open Access Journals (Sweden)

    Jolanta Flieger

    2015-12-01

    Full Text Available A series of imidazolium and pyridinium ionic liquids with different anions (Cl−, Br−, BF4−, PF6− has been evaluated for their adsorption activity on silica gel. Quantification of the ionic liquids has been performed by the use of RP-HPLC with organic-aqueous eluents containing an acidic buffer and a chaotropic salt. Pseudo-second order kinetic models were applied to the experimental data in order to investigate the kinetics of the adsorption process. The experimental data showed good fitting with this model, confirmed by considerably high correlation coefficients. The adsorption kinetic parameters were determined and analyzed. The relative error between the calculated and experimental amount of ionic liquid adsorbed at equilibrium was within 7%. The effect of various factors such as initial ionic liquid concentration, temperature, kind of solvent, kind of ionic liquid anion and cation on adsorption efficiency were all examined in a lab-scale study. Consequently, silica gel showed better adsorptive characteristics for imidazolium-based ionic liquids with chaotropic anions from aqueous solutions in comparison to pyridinium ionic liquids. The adsorption was found to decrease with the addition of organic solvents (methanol, acetonitrile but it was not sensitive to the change of temperature in the range of 5–40 °C.

  3. Identification of the hydrate gel phases present in phosphate-modified calcium aluminate binders

    Energy Technology Data Exchange (ETDEWEB)

    Chavda, Mehul A.; Bernal, Susan A. [Department of Materials Science and Engineering, The University of Sheffield, Sheffield S1 3JD (United Kingdom); Apperley, David C. [Solid-State NMR Group, Department of Chemistry, Durham University, Durham DH1 3LE (United Kingdom); Kinoshita, Hajime [Department of Materials Science and Engineering, The University of Sheffield, Sheffield S1 3JD (United Kingdom); Provis, John L., E-mail: j.provis@sheffield.ac.uk [Department of Materials Science and Engineering, The University of Sheffield, Sheffield S1 3JD (United Kingdom)

    2015-04-15

    The conversion of hexagonal calcium aluminate hydrates to cubic phases in hydrated calcium aluminate cements (CAC) can involve undesirable porosity changes and loss of strength. Modification of CAC by phosphate addition avoids conversion, by altering the nature of the reaction products, yielding a stable amorphous gel instead of the usual crystalline hydrate products. Here, details of the environments of aluminium and phosphorus in this gel were elucidated using solid-state NMR and complementary techniques. Aluminium is identified in both octahedral and tetrahedral coordination states, and phosphorus is present in hydrous environments with varying, but mostly low, degrees of crosslinking. A {sup 31}P/{sup 27}Al rotational echo adiabatic passage double resonance (REAPDOR) experiment showed the existence of aluminium–phosphorus interactions, confirming the formation of a hydrated calcium aluminophosphate gel as a key component of the binding phase. This resolves previous disagreements in the literature regarding the nature of the disordered products forming in this system.

  4. Geology of quartz and hydrated silica-bearing deposits near Antoniadi Crater, Mars

    Science.gov (United States)

    Smith, Matthew R.; Bandfield, Joshua L.

    2012-06-01

    The only area on Mars where crystalline quartz has been identified from orbit is near Antoniadi Crater, on the northern edge of the Syrtis Major shield volcano. However, the method of quartz formation has remained unknown. In this study, we use high-resolution satellite imagery as well as thermal and near-infrared spectroscopy to construct a geologic history of these deposits and their local context. We find that the quartz-bearing deposits are consistently co-located with hydrated silica. This spatial coherence suggests that the quartz formed as a diagenetic product of amorphous silica, rather than as a primary igneous mineral. Diagenetic quartz is a mature alteration product of hydrated amorphous silica, and indicates more persistent water and/or higher temperatures at this site. Beneath the silica-bearing rocks, we also find spectral evidence for smectites in the lowermost exposed Noachian-aged breccia. A similar stratigraphic sequence — smectite-bearing breccias beneath deposits containing minerals suggesting a greater degree of alteration — has also been found at nearby exposures at Nili Fossae and Toro Crater, suggesting a widespread sequence of alteration. By merging the mineral detections of thermal infrared (quartz, feldspar) and near-infrared spectroscopy (hydrated silica, smectite clays) we are able to construct a more complete geologic history from orbit.

  5. Experimental data of inorganic gel based smart window using silica sol–gel process

    Directory of Open Access Journals (Sweden)

    Dayeon Jung

    2016-12-01

    Full Text Available In this article experimental data are presented for inorganic gel based smart window fabricated using silica sol–gel process. Parallel beam transmittances were measured as functions of voltages for samples fabricated with different concentrations of nitric acid. Spectroscopic transmittance data at different driving voltages for samples fabricated with different LC concentrations are shown. Transmittance spectra of the Si–Ti based gel-based-liquid-crystal (GDLC device measured as different driving voltages were compared with those of PDLC. GDLC showed much lower operating voltages, 10–15 V, for on-state. Formation of the LC droplet in gelation process is illustrated. The methyl organic group surrounds LC droplets. Demonstration of GDLC based smart window showed the successful operation with low driving voltages. GDLC window shows clear color, even at off-state, compared with PDLC.

  6. Strength development, hydration reaction and pore structure of autoclaved slag cement with added silica fume

    Energy Technology Data Exchange (ETDEWEB)

    Xi, Y. [China Building Materials Academy, Beijing (China); Siemer, D.D. [LITCO, Idaho Falls, ID (United States); Scheetz, B.E. [Pennsylvania State Univ., University Park, PA (United States). Materials Research Lab.

    1997-01-01

    Under continuous hydrothermal treatment the strength of portland cement paste decreases with curing time and the pore structure coarsens. It was found in this study that the compressive strength of slag cement paste containing 67.5 wt.% ggbfs also decreases with time after 24 hour hydrothermal processing, but with a small addition of silica fume to the slag cement, the cement strength increases and the pore structure densifies when processed under comparable conditions. Based on observations XRD and SEM, these changes are attributed to: (1) changes in the hydration reactions and products by highly reactive silica fume, such that amorphous products dominate and the strength reducing phase {alpha}-C{sub 2}SH does not form; (2) slower hydration of slag, partially caused by the decreased pH of the pore solution, favors the formation of a dense pore structure; and (3) the space filling properties of the micro particles of silica fume.

  7. Sampling tritiated water vapor from the atmosphere by an active system using silica gel

    Energy Technology Data Exchange (ETDEWEB)

    Herranz, M. [Department of Nuclear Engineering and Fluid Mechanics, E.T.S.I. de Bilbao, University of the Basque Country (UPV/EHU), Alameda de Urquijo, s/n 48013 Bilbao (Spain); Alegria, N., E-mail: natalia.alegria@ehu.es [Department of Nuclear Engineering and Fluid Mechanics, E.T.S.I. de Bilbao, University of the Basque Country (UPV/EHU), Alameda de Urquijo, s/n 48013 Bilbao (Spain); Idoeta, R.; Legarda, F. [Department of Nuclear Engineering and Fluid Mechanics, E.T.S.I. de Bilbao, University of the Basque Country (UPV/EHU), Alameda de Urquijo, s/n 48013 Bilbao (Spain)

    2011-11-15

    Among the different methods used to collect the tritiated water vapor (HTO) contained in the atmosphere, one of the most worldwide used is its collection using an air pump, which forces the air to pass through a dry silica gel trap. The silica gel is then distilled to remove the water collected, which is measured in a liquid scintillation counting system. In this paper, an analysis of the water collection efficiency of the silica gel has been done as a function of the temperatures involved, the dimensions of the pipe driving the air into the silica gel traps, the air volume passing through the trap and the flow rates used. Among the obtained conclusions, it can be pointed out that placing the traps inside a cooled container, the amount of silica gel needed to collect all the water contained in the air passing through these traps can be estimated using a weather forecast and a psychometric chart. To do this, and as thermal equilibrium between incoming and open air should be established, a suitable design of the sampling system is proposed. - Highlights: > To recollect the atmosphere air tritiated water vapor, an active system was used. > The system is an air pump and three traps with silica gel connected by a rubber pipe. > The silica gel retention depends on the meteorological conditions and the flow rate. > The amount of water collected and the mass of silica gel need were calculated, F.

  8. A silica sol-gel design strategy for nanostructured metallic materials

    NARCIS (Netherlands)

    Warren, S.C.; Perkins, M.R.; Adams, A.M.; Kamperman, M.M.G.

    2012-01-01

    Batteries, fuel cells and solar cells, among many other high-current-density devices, could benefit from the precise meso- to macroscopic structure control afforded by the silica sol–gel process. The porous materials made by silica sol–gel chemistry are typically insulators, however, which has restr

  9. Effect of silica gel on the cohesion, properties and biological performance of brushite cement.

    Science.gov (United States)

    Alkhraisat, Mohammad Hamdan; Rueda, Carmen; Jerez, Luis Blanco; Tamimi Mariño, Faleh; Torres, Jesus; Gbureck, Uwe; Lopez Cabarcos, Enrique

    2010-01-01

    The cohesion of calcium phosphate cements can be improved by the addition of substances to either the solid or liquid phase during the setting reaction. This study reports the effect of silica gel on brushite cement cohesion. The cement was prepared using a mixture of beta-tricalcium phosphate (beta-TCP) and monocalcium phosphate monohydrate as the solid phase, while the liquid phase comprised carboxylic acids silica gel. This cement presents a shorter final setting time (FST), better cohesion and higher amount of unreacted beta-TCP than the cement prepared without silica gel. Furthermore, in vivo experiments using rabbits as an animal model showed that after 8 weeks of implantation cements modified with silica gel showed a similar new bone formation volume and more remaining graft in comparison with unmodified cements. Thus, the silica gel could be efficiently applied to reduce cement disintegration and to decrease the resorption rate of brushite cements.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-12-29

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

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

    Science.gov (United States)

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

    2015-12-01

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

  12. Crystallization of mixed rare earth (didymium) molybdates in silica gel

    Indian Academy of Sciences (India)

    Sanjay Pandita; Ravender Tickoo; K K Bamzai; P N Kotru; Neera Sahni

    2001-10-01

    Experiments on the growth of mixed rare earth (didymium—a combination of La, Nd, Pr and Sm) molybdates in silica gel medium are reported. The optimum conditions conducive for the growth of these crystals are described and discussed. Concentration programming is reported to enhance the size of crystals by two-fold; the maximum size obtained being about 1 mm3. EDAX results suggest the crystals to be heptamolybdates of type R2Mo7O24, bearing composition La1.23Nd0.43Pr0.29 Sm0.05Mo7O24. The didymium molybdate crystals assume morphologies corresponding to those of spherulites, platelets, cuboids and coalesced crystals. Twinned structure in didymium molybdate crystals are also reported. It is explained that spherulitic morphologies result from aggregates of crystals joining in a spherical envelope. It is suggested that the crystals of didymium molybdates grow by two-dimensional spreading and piling up of layers.

  13. Sol-Gel processing of silica nanoparticles and their applications.

    Science.gov (United States)

    Singh, Lok P; Bhattacharyya, Sriman K; Kumar, Rahul; Mishra, Geetika; Sharma, Usha; Singh, Garima; Ahalawat, Saurabh

    2014-11-06

    Recently, silica nanoparticles (SNPs) have drawn widespread attention due to their applications in many emerging areas because of their tailorable morphology. During the last decade, remarkable efforts have been made on the investigations for novel processing methodologies to prepare SNPs, resulting in better control of the size, shape, porosity and significant improvements in the physio-chemical properties. A number of techniques available for preparing SNPs namely, flame spray pyrolysis, chemical vapour deposition, micro-emulsion, ball milling, sol-gel etc. have resulted, a number of publications. Among these, preparation by sol-gel has been the focus of research as the synthesis is straightforward, scalable and controllable. Therefore, this review focuses on the recent progress in the field of synthesis of SNPs exhibiting ordered mesoporous structure, their distribution pattern, morphological attributes and applications. The mesoporous silica nanoparticles (MSNPs) with good dispersion, varying morphology, narrow size distribution and homogeneous porous structure have been successfully prepared using organic and inorganic templates. The soft template assisted synthesis using surfactants for obtaining desirable shapes, pores, morphology and mechanisms proposed has been reviewed. Apart from single template, double and mixed surfactants, electrolytes, polymers etc. as templates have also been intensively discussed. The influence of reaction conditions such as temperature, pH, concentration of reagents, drying techniques, solvents, precursor, aging time etc. have also been deliberated. These MSNPs are suitable for a variety of applications viz., in the drug delivery systems, high performance liquid chromatography (HPLC), biosensors, cosmetics as well as construction materials. The applications of these SNPs have also been briefly summarized. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Processing, properties, and applications of sol-gel silica optics

    Science.gov (United States)

    Nogues, Jean-Luc R.; LaPaglia, Anthony J.

    1989-12-01

    For many years the market share maintained by U.S. optics manufacturers has been declining continuously caused in part by intense competition principally from countries in the Far East, and in part by the lack of a highly trained cadre of opticians to replace the current generation. This fact could place in jeopardy the defense system of the United States in case of international war. For example, in 1987, optical glass component imports accounted for approximately 50 percent of the Department of Defense (DOD) consumption. GELTECH's sol-gel technology is a new process for making a high quality optical glass and components for commercial and military uses. This technology offers in addition to being a local source of optics, the possibility to create new materials for high-tech optical applications, and the elimination of the major part of grinding and polishing for which the skill moved off-shore. This paper presents a summary of the solgel technology for the manufacture of high quality optical glass and components. Properties of pure silica glass made by solgel process (Type V and Type VI silicas) are given and include: ultraviolet, visible and near infrared spectrophotometry, optical homogeneity and thermal expansion. Many applications such as near net shape casting or Fresnel lens surface replication are discussed. Several potential new applications offered by the solgel technology such as organic-inorganic composites for non linear optics or scintillation detection are also reported in this paper.

  15. Dual-setting brushite-silica gel cements.

    Science.gov (United States)

    Geffers, Martha; Barralet, Jake E; Groll, Jürgen; Gbureck, Uwe

    2015-01-01

    The current study describes a dual-mechanism-setting cement that combines a brushite-forming cement paste with a second inorganic silica-based precursor. Materials were obtained by pre-hydrolyzing tetraethyl orthosilicate (TEOS) under acidic conditions following the addition of a calcium phosphate cement (CPC) powder mixed of β-tricalcium phosphate and monocalcium phosphate. Cement setting occurred by a dissolution-precipitation process, while changes in pH during setting simultaneously initiated the condensation reaction of the hydrolyzed TEOS. This resulted in an interpenetrating phase composite material in which the macropores of the CPC were infiltrated by the microporous silica gel, leading to a higher density and a compressive strength ∼5-10 times higher than the CPC reference. This also altered the release of vancomycin as a model drug, whereby in contrast to the quantitative release from the CPC reference, 25% of the immobilized drug remained in the composite matrix. By varying the TEOS content in the composite, the cement phase composition could be controlled to form either brushite, anhydrous monetite or a biphasic mixture of both. The composites with the highest silicate content showed a cell proliferation similar to a hydroxyapatite reference with a significantly higher activity per cell. Surprisingly, the biological response did not seem to be attributed to the released silicate ions, but to the release of phosphate and the adsorption of magnesium ions from the cell culture medium.

  16. A Novel Approach for Entrapment of Biopolymers in Silica Matrix by Sol-gel Technique

    Institute of Scientific and Technical Information of China (English)

    Yu.Shchipunov

    2007-01-01

    1 Results The entrapment of biopolymers into silica by the sol-gel technique meets with incompatibility of inorganic and bioorganic components. The aim was to develop a compatible procedure biomimicking the biomineralization processes in the living nature. A suggested solution in Ref.[1-2] for the biopolymer entrapment into silica matrix is based on a novel silica precursor. The developed approach is distinguished from the common technique for fabrication of hybrid biopolymer-silica nanocomposite materi...

  17. Synthesis of Titania-Silica Materials by Sol-Gel

    Directory of Open Access Journals (Sweden)

    Rubia F. S. Lenza

    2002-10-01

    Full Text Available In this work TiO2-SiO2 glasses containing as much as 20 mol % of TiO2 were prepared via sol-gel process using titanium and silicon alkoxides, in the presence of chlorine, in the form of titanium tetrachloride or HCl. The gels were heat-treated until 800 °C. X-ray diffraction and Fourier transform infrared spectroscopy were used to understand the structural properties of TiO2-SiO2 oxides calcined at different temperatures and to evaluate the homogeneity of these materials. The degree of the compactness of the silica network is inferred from the frequency of the asymmetric stretching vibrations of Si-O-Si bonds. Formation of Si-O-Ti bridges, as monitored by the intensity of characteristic 945 cm-1 ¾ 960 cm-1 vibration, is particularly prominent if the method of basic two-step prehydrolysis of silicon alkoxide, addition of titanium alkoxide and completion of hydrolysis was used.

  18. Formation of macroporous gel morphology by phase separation in the silica sol-gel system containing nonionic surfactant

    Institute of Scientific and Technical Information of China (English)

    Junsheng Wu; Xiaogang Li; Wei Du; Hua Chen

    2005-01-01

    The phase separation and gel formation behavior in an alkoxy-derived silica sol-gel system containing Ci6EOi5 has been investigated. Various gel morphologies similar to other sol-gel systems containing organic additives were obtained by changing the preparation conditions. Micrometer-range interconnected porous gels were obtained by freezing transitional structures of phase separation in the sol-gel process. The dependence of the resulting gel morphology on several important reaction parameters such as the starting composition, reaction temperature and acid catalyst concentration was studied in detail. The experimental results indicate that the gel morphology is mainly determined by the time relation between the onset of phase separation and gel formation.

  19. Radiation hardening in sol-gel derived Er{sup 3+}-doped silica glasses

    Energy Technology Data Exchange (ETDEWEB)

    Hari Babu, B., E-mail: hariphy2012@gmail.com, E-mail: matthieu.lancry@u-psud.fr; León Pichel, Mónica [Laboratoire des Solides Irradiés, UMR CEA-CNRS 7642, Ecole Polytechnique, Université Paris Saclay, 91128 Palaiseau (France); Institut de Chimie Moléculaire et des Matériaux d' Orsay, UMR CNRS-UPSud 8182, Université Paris Sud, 91405 Orsay (France); Ollier, Nadège [Laboratoire des Solides Irradiés, UMR CEA-CNRS 7642, Ecole Polytechnique, Université Paris Saclay, 91128 Palaiseau (France); El Hamzaoui, Hicham; Bigot, Laurent; Savelii, Inna; Bouazaoui, Mohamed [Laboratoire PhLAM (UMR CNRS 8523), IRCICA (USR CNRS 3380), CERLA - FR CNRS 2416, Université Lille 1, Villeneuve d' Ascq Cedex F-59655 (France); Poumellec, Bertrand; Lancry, Matthieu, E-mail: hariphy2012@gmail.com, E-mail: matthieu.lancry@u-psud.fr [Institut de Chimie Moléculaire et des Matériaux d' Orsay, UMR CNRS-UPSud 8182, Université Paris Sud, 91405 Orsay (France); Ibarra, Angel [National Fusion Laboratory, CIEMAT, Avda Complutense 40, 28040 Madrid (Spain)

    2015-09-28

    The aim of the present paper is to report the effect of radiation on the Er{sup 3+}-doped sol-gel silica glasses. A possible application of these sol-gel glasses could be their use in harsh radiation environments. The sol-gel glasses are fabricated by densification of erbium salt-soaked nanoporous silica xerogels through polymeric sol-gel technique. The radiation-induced attenuation of Er{sup 3+}-doped sol-gel silica is found to increase with erbium content. Electron paramagnetic resonance studies reveal the presence of E′{sub δ} point defects. This happens in the sol-gel aluminum-silica glass after an exposure to γ-rays (kGy) and in sol-gel silica glass after an exposure to electrons (MGy). The concentration levels of these point defects are much lower in γ-ray irradiated sol-gel silica glasses. When the samples are co-doped with Al, the exposure to γ-ray radiation causes a possible reduction of the erbium valence from Er{sup 3+} to Er{sup 2+} ions. This process occurs in association with the formation of aluminum oxygen hole centers and different intrinsic point defects.

  20. Effect of Fly Ash and Silica Fume on Hydration Rate of Cement Pastes and Strength of Mortars

    Institute of Scientific and Technical Information of China (English)

    LIU Jun; ZHANG Yun; LIU Runqing; ZHANG Bing

    2014-01-01

    The effect of fly ash and silica fume on hydration rate and strength of cement in the early stage was studied. Contrast test was applied to the complex cementitious system to investigate the hydration rate. Combined with mechanical strength, the influence of fly ash and silica fume during the hydration process of complex binder was researched. The peak of the rate of hydration heat evolution and the mechanical strength decreased as the ratio of fly ash increased, however, as the ratio of silica fume increased, the peak of the rate of hydration heat evolution and the mechanical strength increased obviously. When the ratios of fly ash and silica fume are 10%and 5%, the peak of the rate of hydration heat evolution is the highest. At the same time 7 days of flexural and compressive strength are the highest as 8.89 MPa and 46.52 MPa, respectively. Fly ash and silica fume are the main factors affecting the hydration rate and the mechanical property.

  1. Fabrication of SWNT/silica composites by the sol-gel process.

    Science.gov (United States)

    Babooram, Keshwaree; Narain, Ravin

    2009-01-01

    Single-walled carbon nanotubes (SWNTs) have successfully been incorporated into a silica matrix using the sol-gel process. The SWNTs were first functionalized with 3-aminopropyltriethoxysilane (APTES) through an amide linkage formed between the carboxylic acid groups already present on their surface and the amino group on APTES. The silane moieties were then used to form silica with and without the presence of tetramethylorthosilicate (TMOS) in a sol-gel reaction. The addition of TMOS was found to influence the molecular arrangement of the SWNT in the silica matrix and also to retard the degradation of the silica-SWNT composite.

  2. Palladium Immobilized on Silica Gel: A Novel and Reusable Catalyst for Heck Reaction

    Institute of Scientific and Technical Information of China (English)

    WANG Zu-Li; WANG Lei; YAN Jin-Can

    2008-01-01

    The immobilization of palladium on silica gel in Heck reaction has been developed.Iodobenzenes,bromobenzenes and activated chlorobenzenes were coupled with olefins (Heck reaction) smoothly to afford the corresponding cross-coupling products in good to excellent yields under phosphine- and amine-free reaction conditions in the presence of silica gel supported palladium,Silica-Ap-Pd cat.as catalyst,potassium carbonate as base and DMF as solvent.Furthermore,the silica-supported palladium catalyst 3 could be recovered and recycled by a simple filtration of the reaction solution and used for 6 consecutive trials without significant loss of its catalytic activity.

  3. A facile one-pot synthesis of ruthenium hydroxide nanoparticles on magnetic silica: Aqueous hydration of nitriles to amides

    Science.gov (United States)

    One-pot synthesis of ruthenium hydroxide nanoparticles on magnetic silica is described which involve the in situ generation of magnetic silica (Fe3O4@ SiO2) and ruthenium hydroxide immobilization; the hydration of nitriles occurs in high yield and excellent selectivity using this...

  4. A facile one-pot synthesis of ruthenium hydroxide nanoparticles on magnetic silica: Aqueous hydration of nitriles to amides

    Science.gov (United States)

    One-pot synthesis of ruthenium hydroxide nanoparticles on magnetic silica is described which involve the in situ generation of magnetic silica (Fe3O4@ SiO2) and ruthenium hydroxide immobilization; the hydration of nitriles occurs in high yield and excellent selectivity using this...

  5. Dermal tolerance and effect on skin hydration of a new ethanol-based hand gel.

    Science.gov (United States)

    Kampf, G; Muscatiello, M; Häntschel, D; Rudolf, M

    2002-12-01

    We studied the dermal tolerance (repetitive occlusive patch test; ROPT) and the skin hydrating properties of a new ethanol-based gel [85% (w/w)], Sterillium Gel. For the ROPT, 53 participants were studied. Gel was applied to one site on the back under an occlusive patch during an induction phase (nine applications over three weeks) and two weeks later to a virgin site on the back during a challenge phase (one application). Twenty-four hours after the removal of the patches (induction phase and challenge phase), then 48 and 72 h later (challenge phase) sites were graded for skin reactions using a standardized scale. In the induction phase none of the 53 participants had a skin reaction. In the challenge phase one participant had a barely perceptible skin reaction, and one had mild erythema at one time point. To evaluate skin hydrating properties of the gel, treated skin of 21 participants was compared to untreated skin. The gel was applied twice a day to the forearm for 14 days. Control corneometer values were taken before application of the gel (mean: 32.7 +/- 5.0) and after one (36.3 +/- 4.4) and two weeks (36.1 +/- 5.4). Relative skin hydration on treated skin in comparison with an untreated control field was significantly higher after one week by 6.85% (P = 0.0031; paired t -test for dependent samples) and after two weeks by 4.47% (P = 0.0153). Sterillium Gel did not demonstrate a clinically relevant potential for dermal irritation or sensitization, and significantly increased skin hydration after repetitive use, and so could enhance compliance with hand hygiene among healthcare workers.

  6. Kinetics of hydrate formation and decomposition of methane in silica sand

    Energy Technology Data Exchange (ETDEWEB)

    Nam, S.C. [Korea Inst. of Energy Reserch, Daejeon (Korea, Republic of). Dept. of Energy Conversion Research; Linga, P.; Haligva, C.; Englezos, P. [British Columbia Univ., Vancouver, BC (Canada). Dept. of Chemical and Biological Engineering; Ripmeester, J.A. [National Research Council of Canada, Ottawa, ON (Canada). Steacie Inst. for Molecular Sciences

    2008-07-01

    The kinetics of hydrate formation and the decomposition behaviour of methane hydrates formed in a bed of silica sand particles were investigated. An experimental apparatus was used to study hydrate formation at temperatures of 7.0, 4.0, and 1.0 degrees C. Thermocouples were used to obtain temperature profiles during the experiments. Data obtained from the experiments were then used to determine formation gas uptake measurement curves and gas release decomposition measurement curves. Results of the study showed that the percentage of water converted to hydrates was higher when the temperature was 1.0 degrees C. Multiple nucleation points occurred during formation experiments conducted at 4.0 and 1.0 degrees C. A thermal stimulation approach was used to recover methane from the hydrates. The study showed that methane recovery occurred during 2 stages of the decomposition process. It was concluded that methane recovery rates of between 95 and 98 per cent were achieved using the method. 35 refs., 6 figs.

  7. Analysis of the retention of water vapor on silica gel; Analisis de la retencion del vapor de agua en silica gel

    Energy Technology Data Exchange (ETDEWEB)

    Herranz, M.; Pinilla, J. L.; Alegria, N.; Idoeta, R.; Legarda, F.

    2011-07-01

    Among the various sampling systems tritium content in the atmosphere as water vapor, one of the most basic and, therefore, of widespread use in the environmental field, is the retention on silica gel. However, the behavior of the collection efficiency of silica gel under varying conditions of air temperature and relative humidity makes it difficult to define the amount of this necessary for proper completion of sampling, especially in situations of prolonged sampling. This paper presents partial results obtained in a study on the analysis of these efficiencies under normal conditions of sampling. (Author)

  8. RHEOLOGICAL MODIFICATION OF EPOXY RESINS WITH NANO SILICA PREPARED BY THE SOL-GEL PROCESS

    Institute of Scientific and Technical Information of China (English)

    Xia Wang; Jiang Li; Cheng-fen Long; Yun-zhao Yu

    1999-01-01

    Nano silica-modified epoxy resins were synthesized by the sol-gel process. The materials have the morphological structure of nano particales dispersed in the epoxy matrix. The dispersed phase formed a physical network in the resin and thus influenced the rheological behavior greatly. However, the nano silica did not show a significant influence on the mechanical properties of the cured resins.

  9. The Role Seemingly of Amorphous Silica Gel Layers in Chiral Separations by Planar Chromatography

    Directory of Open Access Journals (Sweden)

    Teresa Kowalska

    2007-12-01

    Full Text Available In planar chromatography, silica gel appears as the most frequently used adsorbent. Its preference as planar chromatographic stationary phase is due to its high specific surface area (ca. 700 m2 g-1 and relatively simple active sites (silanol groups, Si-OH. The high specific surface area of silica gel and a high density of coverage of its surface with the silanol active sites contribute jointly to an excellent separation performance of this adsorbent. In our experiments on chiral separation of the enantiomer pairs by planar chromatography, contradictory behavior of the silica gel layers versus the chiral compounds was observed. The migration tracks of chiral compounds in the ascending planar chromatographic mode were not vertical but bent on either side being a function of analyte chirality. This deviation of the analyte’s migration track was noticed, when using the densitometric scanner to quantify the respective chromatograms. In order to confirm the hypothesis as to the microcrystalline nature of silica gel used in liquid chromatography, it was further investigated through circular dichroism (CD and the data thereof confirmed that the ‘chromatographic’ silica gels are not amorphous but microcrystalline, contributing to the (partial horizontal enantioseparation of the antimer pairs. This paper summarizes the results of our investigation on the microcrystalline nature of silica gels used in planar chromatography and their impact on enantioseparation of the selected pairs of antimers.

  10. Rice Husk Ash as a Renewable Source for the Production of Value Added Silica Gel and its Application: An Overview

    Directory of Open Access Journals (Sweden)

    Ram Prasad

    2012-06-01

    Full Text Available In recent years, silica gels have developed a lot of interest due to their extraordinary properties and their existing and potential applications in science and technology. Silica gel has a wide range of applications such as a desiccant, as a preservation tool to control humidity, as an adsorbent, as a catalyst and as a cata-lyst support. Silica gel is a rigid three-dimensional network of colloidal silica, and is classified as: aqua-gel, alco-gel, xero-gel and aero-gel. Out of all known solid porous materials, aero-gels are particularly known for their high specific surface area, high porosity, low bulk density, high thermal insulation value, ultra low dielectric constant and low index of refraction. Because of these extraordinary properties silica aero-gel has many commercial applications such as thermal window insulation, acoustic barriers, super-capacitors and catalytic supports. However, monolithic silica aero-gel has been used extensively in high energy physics in Cherenkov radiation detectors and in shock wave studies at high pressures, inertial confinement fusion (ICF radio-luminescent and micrometeorites. Silica gel can be prepared by using various sol gel precursors but the rice husk (RH is considered as the cheapest source for silica gel production. Rice husk is a waste product abundantly available in rice producing countries during milling of rice. This review article aims at summarizing the developments carried out so far in synthesis, properties, characterization and method of determination of silica, silica gel, silica aero-gel and silica xero-gel. The effect of synthesis parameters such as pH, temperature of burning the rice husk, acid leaching prior to formation of rice husk ash (RHA on the properties of final product are also described. The attention is also paid on the application of RH, RHA, sil-ica, silica aero-gel and silica xero-gel. Development of economically viable processes for getting rice husk silica with specific

  11. Cement with silica fume and granulated blast-furnace slag: strength behavior and hydration

    Directory of Open Access Journals (Sweden)

    Bonavetti, V. L.

    2014-09-01

    Full Text Available This paper analyses the influence of portland cement replacement by silica fume (up to 10% and/or granulated blast furnace slag (up to 70% on the hydration cement (XRD, heat of hydration, non evaporable water content and calcium hydroxide content curing under sealed conditions and their effect on the mechanical strength. The obtained results indicate that binary cements containing silica fume and ternary cements there was a significant increase of hydration rate at early age. At later ages, most of studied cements have an equivalent or greater strength that those obtained in the plain portland cement.En este trabajo se analiza la influencia de la incorporación al cemento portland de humo de sílice (hasta 10% y/o escoria granulada de alto horno (hasta 70% sobre la hidratación (DRX, calor de hidratación, contenido de agua no evaporable y de hidróxido de calcio, bajo condiciones de curado sellado y su incidencia sobre la resistencia mecánica. Los resultados obtenidos indican que en los cementos binarios con humo de sílice y en los cementos ternarios se produce un importante aumento de la velocidad de hidratación en las primeras edades, mientras que a edades más avanzadas la mayor parte del dominio estudiado alcanza o supera la resistencia obtenida por el cemento portland sin adición.

  12. Sol-gel silica films embedding NIR- emitting Yb-quinolinolate complexes

    Energy Technology Data Exchange (ETDEWEB)

    Figus, Cristiana, E-mail: cristiana.figus@dsf.unica.it; Quochi, Francesco, E-mail: cristiana.figus@dsf.unica.it; Piana, Giacomo; Saba, Michele; Mura, Andrea; Bongiovanni, Giovanni [Dipartimento di Fisica, University of Cagliari, SS 554 Bivio per Sestu, I-09042, Monserrato-Cagliari (Italy); Artizzu, Flavia [Dipartimento di Fisica, University of Cagliari and Dipartimento di Scienze Chimiche e Geologiche, University of Cagliari, SS 554 Bivio per Sestu, I-09042, Monserrato-Cagliari (Italy); Mercuri, Maria Laura; Serpe, Angela; Deplano, Paola [Dipartimento di Scienze Chimiche e Geologiche, University of Cagliari, SS 554 Bivio per Sestu, I-09042, Monserrato-Cagliari (Italy)

    2014-10-21

    Sol-gel silica thin films embedding an ytterbium quinolinolato complex (YbClQ{sub 4}) have been obtained using different alkoxides. Homogeneous, crack- and defect-free thin films of optical quality have been successfully deposited on glass substrate by dip-coating. The silica thin films have been characterized by time-resolved photoluminescence. The luminescence properties of the YbClQ{sub 4} are preserved in silica films prepared through an optimized sol-gel approach. The excited state lifetime of the lanthanide is comparable to those observed in bulk and longer than the corresponding ones in solution.

  13. Sol-gel silica films embedding NIR- emitting Yb-quinolinolate complexes

    Science.gov (United States)

    Figus, Cristiana; Quochi, Francesco; Artizzu, Flavia; Piana, Giacomo; Saba, Michele; Mercuri, Maria Laura; Serpe, Angela; Deplano, Paola; Mura, Andrea; Bongiovanni, Giovanni

    2014-10-01

    Sol-gel silica thin films embedding an ytterbium quinolinolato complex (YbClQ4) have been obtained using different alkoxides. Homogeneous, crack- and defect-free thin films of optical quality have been successfully deposited on glass substrate by dip-coating. The silica thin films have been characterized by time-resolved photoluminescence. The luminescence properties of the YbClQ4 are preserved in silica films prepared through an optimized sol-gel approach. The excited state lifetime of the lanthanide is comparable to those observed in bulk and longer than the corresponding ones in solution.

  14. Phase separation during silica gel formation followed by time-resolved SAXS

    Energy Technology Data Exchange (ETDEWEB)

    Gommes, Cedric J. [Universite de Liege, Laboratoire de Genie Chimique, Bat B6a, Allee du 6 aout 3, B-4000 Sart Tilman Liege (Belgium)]. E-mail: cedric.gommes@ulg.ac.be; Blacher, Silvia [Universite de Liege, Laboratoire de Genie Chimique, Bat B6a, Allee du 6 aout 3, B-4000 Sart Tilman Liege (Belgium); Goderis, Bart [Katholieke Universiteit Leuven, Laboratorium voor Macromoleculaire Structuurchemie, Celestijnenlann 200F, B-3001 Heverlee (Belgium); Pirard, Jean-Paul [Universite de Liege, Laboratoire de Genie Chimique, Bat B6a, Allee du 6 aout 3, B-4000 Sart Tilman Liege (Belgium)

    2005-08-15

    Time-resolved small angle X-ray scattering data are collected during the formation of silica gels from the base catalyzed polymerization of tetraethoxysilane in ethanol with 3-(2-aminoethylamino)propyltrimethoxysilane and 3-aminopropyltriethoxysilane as additives. It is shown that a polymerization-induced spinodal demixing occurs during the gel formation.

  15. An Experimental Study of the Liesegang Phenomenon and Crystal Growth in Silica Gels.

    Science.gov (United States)

    Sharbaugh, Amandus H., III; Sharbaugh, Amandus H., Jr.

    1989-01-01

    Reports on a 30-year-old longitudinal study of reactions in gels. Described are reactions and crystal growth in silica gels and diffusion studies of the Liesegang ring formation. Color photographs showing the reactions and graphs upon the diffusions are presented. (YP)

  16. Effect of hydration on the structure of non aqueous ethyl cellulose/propylene glycol dicaprylate gels.

    Science.gov (United States)

    Bruno, Lilia; Kasapis, Stefan; Heng, Paul W S

    2012-03-01

    Changes in the structural properties of ethyl cellulose/propylene glycol dicaprylate systems (EC/PGD), intended for topical drug delivery, upon addition of water were investigated. Although designed to be a non-aqueous vehicle for moisture sensitive drugs, these systems are expected to experience an aqueous environment during production, storage and application on the skin. Hence, the interaction of water molecules with the non aqueous gel system and their distribution within the gel network is of interest and critical to its application. Experimental techniques of this study were small-deformation dynamic oscillation in shear, modulated differential scanning calorimetry (MDSC), (2)H NMR spectroscopy, ATR-infrared spectroscopy, wide-angle X-ray diffraction patterns and light microscopy. Rheological profiles of the gels containing moisture from 0.1 to 40.0% (w/w) deviated considerably from that of the non aqueous system at levels of water above 10.0% in preparations. Gradual replacement of the EC/PGD dipole interactions with stronger hydrogen bonding between ethyl cellulose chains, as the level of hydration increased, contributed to these observations. Formation of clusters of ethyl cellulose, observed under a light microscope, was thus ensued. X-ray diffraction patterns showed that the rearrangement of the polymer chains led to the loss of liquid crystal structures found in the anhydrous gel. MDSC and (2)H NMR were used to further shed light on the thermodynamic state of added water molecules in the gels. Plots of enthalpy obtained calorimetrically and a good correlation between MDSC and (2)H NMR data indicate that gels with less than two percent hydration contain water in a non-freezable bound state, whereas freezable moieties are obtained at levels of hydration above five percent in composite (EC/PGD/water) gels.

  17. Gel-based composite polymer electrolytes with novel hierarchical mesoporous silica network for lithium batteries

    Energy Technology Data Exchange (ETDEWEB)

    Wang Xiaoliang; Cai Qiang [Department of Materials Science and Engineering, and State Key Laboratory of New Ceramics and Fine Processing, Tsinghua University, Beijing 100084 (China); Fan Lizhen [School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083 (China); Hua Tao; Lin Yuanhua [Department of Materials Science and Engineering, and State Key Laboratory of New Ceramics and Fine Processing, Tsinghua University, Beijing 100084 (China); Nan Cewen [Department of Materials Science and Engineering, and State Key Laboratory of New Ceramics and Fine Processing, Tsinghua University, Beijing 100084 (China)], E-mail: cwnan@tsinghua.edu.cn

    2008-11-15

    In the present work, novel gel-based composite polymer electrolytes for lithium batteries were prepared by introducing a hierarchical mesoporous silica network to the poly(vinylidene fluoride-hexafluoropropylene) (PVDF-HFP)-based gel electrolytes. As compared with the PVDF-HFP-based gel electrolytes with/without conventional nano-sized silica fillers, the novel electrolytes have shown more homogeneous microstructure, higher ionic conductivity and better mechanical stability, which could be caused by the strong silica network and the effective interactions among the polymer, the liquid electrolytes and the silica. Moreover, the cell with this kind of electrolytes could achieve a discharge capacity as much as 150 mAh g{sup -1} at room temperature (LiCoO{sub 2} as the cathode active material), with high Coulomb efficiency.

  18. Gel-based composite polymer electrolytes with novel hierarchical mesoporous silica network for lithium batteries

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Xiao-Liang; Cai, Qiang; Hua, Tao; Lin, Yuan-Hua; Nan, Ce-Wen [Department of Materials Science and Engineering, and State Key Laboratory of New Ceramics and Fine Processing, Tsinghua University, Beijing 100084 (China); Fan, Li-Zhen [School of Materials Science and Engineering, University of Science and Technology Beijing, Beijing 100083 (China)

    2008-11-15

    In the present work, novel gel-based composite polymer electrolytes for lithium batteries were prepared by introducing a hierarchical mesoporous silica network to the poly(vinylidene fluoride-hexafluoropropylene) (PVDF-HFP)-based gel electrolytes. As compared with the PVDF-HFP-based gel electrolytes with/without conventional nano-sized silica fillers, the novel electrolytes have shown more homogeneous microstructure, higher ionic conductivity and better mechanical stability, which could be caused by the strong silica network and the effective interactions among the polymer, the liquid electrolytes and the silica. Moreover, the cell with this kind of electrolytes could achieve a discharge capacity as much as 150 mAh g{sup -1} at room temperature (LiCoO{sub 2} as the cathode active material), with high Coulomb efficiency. (author)

  19. Preparation and characterization of silk/silica hybrid biomaterials by sol-gel crosslinking process

    Energy Technology Data Exchange (ETDEWEB)

    Hou Aiqin, E-mail: aiqinhou@dhu.edu.c [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China); Chen Huawei [National Engineering Research Center for Dyeing and Finishing of Textiles, Donghua University, 3H, 2999 North Renmin Road, Songjiang, Shanghai 201620 (China)

    2010-03-15

    The silk/silica hybrid biomaterials are synthesized by sol-gel crosslinking process. The chemical and morphological structures of silk/silica hybrids are investigated with micro-FT-IR spectra, X-ray diffraction, SEM, AFM, and DSC. The results show that the crosslinking reactions among inorganic nano-particles, fibroin and 2,4,6-tri[(2-epihydrin-3-bimethyl-ammonium)propyl]-1,3,5-triazine chloride (Tri-EBAC) take place during sol-gel process. The silk/silica hybrids form new molecular structures containing not only organic fibroin but also inorganic nano-silica particles. The inorganic particles are bounded to the fibroin through covalent bonds. The silk/silica hybrids can form excellent film with very even nanometer particles. The thermal properties of organic/inorganic hybrid are improved.

  20. A silica sol-gel design strategy for nanostructured metallic materials.

    Science.gov (United States)

    Warren, Scott C; Perkins, Matthew R; Adams, Ashley M; Kamperman, Marleen; Burns, Andrew A; Arora, Hitesh; Herz, Erik; Suteewong, Teeraporn; Sai, Hiroaki; Li, Zihui; Werner, Jörg; Song, Juho; Werner-Zwanziger, Ulrike; Zwanziger, Josef W; Grätzel, Michael; DiSalvo, Francis J; Wiesner, Ulrich

    2012-03-18

    Batteries, fuel cells and solar cells, among many other high-current-density devices, could benefit from the precise meso- to macroscopic structure control afforded by the silica sol-gel process. The porous materials made by silica sol-gel chemistry are typically insulators, however, which has restricted their application. Here we present a simple, yet highly versatile silica sol-gel process built around a multifunctional sol-gel precursor that is derived from the following: amino acids, hydroxy acids or peptides; a silicon alkoxide; and a metal acetate. This approach allows a wide range of biological functionalities and metals--including noble metals--to be combined into a library of sol-gel materials with a high degree of control over composition and structure. We demonstrate that the sol-gel process based on these precursors is compatible with block-copolymer self-assembly, colloidal crystal templating and the Stöber process. As a result of the exceptionally high metal content, these materials can be thermally processed to make porous nanocomposites with metallic percolation networks that have an electrical conductivity of over 1,000 S cm(-1). This improves the electrical conductivity of porous silica sol-gel nanocomposites by three orders of magnitude over existing approaches, opening applications to high-current-density devices.

  1. Nanoscale Charge Balancing Mechanism in Alkali Substituted Calcium-Silicate-Hydrate Gels

    CERN Document Server

    Özçelik, V Ongun

    2016-01-01

    Alkali-activated materials and related alternative cementitious systems are sustainable material technologies that have the potential to substantially lower CO$_2$ emissions associated with the construction industry. However, the impact of augmenting the chemical composition of the material on the main binder phase, calcium-silicate-hydrate gel, is far from understood, particularly since this binder phase is disordered at the nanoscale. Here, we reveal the presence of a charge balancing mechanism at the molecular level, which leads to stable structures when alkalis (i.e., Na or K) are incorporated into a calcium-silicate-hydrate gel, as modeled using crystalline 14{\\AA} tobermorite. These alkali containing charge balanced structures possess superior mechanical properties compared to their charge unbalanced counterparts. Our results, which are based on first-principles simulations using density functional theory, include the impact of charge balancing on the optimized geometries of the new model phases, format...

  2. Radiation hardening of sol gel-derived silica fiber preforms through fictive temperature reduction.

    Science.gov (United States)

    Hari Babu, B; Lancry, Matthieu; Ollier, Nadege; El Hamzaoui, Hicham; Bouazaoui, Mohamed; Poumellec, Bertrand

    2016-09-20

    The impact of fictive temperature (Tf) on the evolution of point defects and optical attenuation in non-doped and Er3+-doped sol-gel silica glasses was studied and compared to Suprasil F300 and Infrasil 301 glasses before and after γ-irradiation. To this aim, sol-gel optical fiber preforms have been fabricated by the densification of erbium salt-soaked nanoporous silica xerogels through the polymeric sol-gel technique. These γ-irradiated fiber preforms have been characterized by FTIR, UV-vis-NIR absorption spectroscopy, electron paramagnetic resonance, and photoluminescence measurements. We showed that a decrease in the glass fictive temperature leads to a decrease in the glass disorder and strained bonds. This mainly results in a lower defect generation rate and thus less radiation-induced attenuation in the UV-vis range. Furthermore, it was found that γ-radiation "hardness" is higher in Er3+-doped sol-gel silica compared to un-doped sol-gel silica and standard synthetic silica glasses. The present work demonstrates an effective strategy to improve the radiation resistance of optical fiber preforms and glasses through glass fictive temperature reduction.

  3. Silica-rich deposits and hydrated minerals at Gusev Crater, Mars: Vis-NIR spectral characterization and regional mapping

    Science.gov (United States)

    Rice, M.S.; Bell, J.F.; Cloutis, E.A.; Wang, A.; Ruff, S.W.; Craig, M.A.; Bailey, D.T.; Johnson, J. R.; De Souza, P.A.; Farrand, W. H.

    2010-01-01

    The Mars Exploration Rover (MER) Spirit has discovered surprisingly high concentrations of amorphous silica in soil and nodular outcrops in the Inner Basin of the Columbia Hills. In Pancam multispectral observations, we find that an absorption feature at the longest Pancam wavelength (1009 nm) appears to be characteristic of these silica-rich materials; however, spectral analyses of amorphous silica suggest that the ???1009 nm spectral feature is not a direct reflection of their silica-rich nature. Based on comparisons with spectral databases, we hypothesize that the presence of H2O or OH, either free (as water ice), adsorbed or bound in a mineral structure, is responsible for the spectral feature observed by Pancam. The Gertrude Weise soil, which is nearly pure opaline silica, may have adsorbed water cold-trapped on mineral grains. The origin of the ???1009 nm Pancam feature observed in the silica-rich nodular outcrops may result from the presence of additional hydrated minerals (specific sulfates, halides, chlorides, sodium silicates, carbonates or borates). Using the ???1009 nm feature with other spectral parameters as a "hydration signature" we have mapped the occurrence of hydrated materials along the extent of Spirit's traverse across the Columbia Hills from West Spur to Home Plate (sols 155-1696). We have also mapped this hydration signature across large panoramic images to understand the regional distribution of materials that are spectrally similar to the silica-rich soil and nodular outcrops. Our results suggest that hydrated materials are common in the Columbia Hills. ?? 2009 Elsevier Inc.

  4. Preparation of an efficient humidity indicating silica gel from rice husk ash

    Indian Academy of Sciences (India)

    J P Nayak; J Bera

    2011-12-01

    An efficient humidity indicating silica gel was prepared using rice husk ash as a raw material via sodium silicate extraction and acid neutralization method. Cobalt chloride was impregnated into the silica gel as a colour indicating material. A low concentration of cobalt chloride solution (0.0005 mol dm-3) was used for the impregnation. The effect of pH of the impregnating solution on the colour development behaviour of the gel was investigated. The specific surface area of the gel was determined by Brunauer–Emmett–Teller method. The gel has been characterized using X-ray diffraction, scanning electron microscopy and visible spectroscopy. The moisture adsorption and desorption kinetics of the desiccant were evaluated using simultaneous thermogravimetry and differential scanning calorimetry.

  5. Styrene grafted natural rubber reinforced by in situ silica generated via sol–gel technique

    Energy Technology Data Exchange (ETDEWEB)

    Sittiphan, Torpong [Program of Petrochemistry and Polymer Sciences, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Prasassarakich, Pattarapan [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand); Poompradub, Sirilux, E-mail: sirilux.p@chula.ac.th [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Bangkok 10330 (Thailand)

    2014-02-15

    Highlights: • Sol–gel reaction by NR latex was the absence of use of organic solvent and base catalyst. • Well dispersed in situ formed silica particles in the rubber matrix were obtained. • In situ silica was better to improve mechanical properties of rubber vulcanizates. -- Abstract: The filling of styrene graft natural rubber (ST-GNR) with in situ formed silica was performed using the sol–gel reaction via the latex solution method. The mechanical properties of ST-GNR/NR vulcanizate were improved when using the in situ formed silica to levels higher than those obtained with the commercial ex situ formed silica filled ST-GNR/NR vulcanizates at a comparable silica content of 12 parts by weight per hundred parts of rubber. Transmission electron microscopy analysis revealed that the in situ silica particles were small (∼40 nm diameter) and well dispersed, while the commercial silica particles were larger (∼60 nm diameter) and markedly agglomerated in the rubbery matrix. The mechanical properties of the composites prepared via both the solid rubber and latex solution methods were comparable.

  6. Preparation and Characterization of Kynurenic Acid Occluded in Sol-Gel Silica and SBA-15 Silica as Release Reservoirs

    Directory of Open Access Journals (Sweden)

    Tessy López

    2014-01-01

    Full Text Available Kynurenic acid (KYNA may have important therapeutic effects in neurological disorders; however, its use as a neuroprotective agent is restricted due to its very limited ability to cross the blood brain barrier (BBB. For this reason, we are looking for new alternatives for KYNA to reach the brain; one of them is using drug delivery systems. To obtain KYNA release reservoirs, KYNA molecules were hosted in two different silica materials. The different KYNA-silica materials were characterized by means of several physical techniques. The spectroscopic studies showed that KYNA molecules remained unchanged once hosted in silica materials. The surface area values of KYNA-silica samples were substantially lower than those for pure silica materials due to the addition of the drug. The electronic micrographs showed that the sol-gel KYNA-silica material consisted of aggregates of nanoparticles around 50 nm in size. On the other hand, the typical SBA-15 hexagonal arrangement was observed, even when hosting KYNA molecules. KYNA release profiles, carried out during approximately 300 hours, showed a first stage of fast drug release followed by a slow release phase. The experimental values fitted to the Peppas equation indicate that the release mechanism was controlled by Fickian diffusion.

  7. Tailoring the oxidation state of cobalt through halide functionality in sol-gel silica

    OpenAIRE

    Gianni Olguin; Christelle Yacou; Simon Smart; Diniz da Costa, João C.

    2013-01-01

    The functionality or oxidation state of cobalt within a silica matrix can be tailored through the use of cationic surfactants and their halide counter ions during the sol-gel synthesis. Simply by adding surfactant we could significantly increase the amount of cobalt existing as Co3O4 within the silica from 44% to 77%, without varying the cobalt precursor concentration. However, once the surfactant to cobalt ratio exceeded 1, further addition resulted in an inhibitory mechanism whereby the alt...

  8. Dynamic impact indentation of hydrated biological tissues and tissue surrogate gels

    Science.gov (United States)

    Ilke Kalcioglu, Z.; Qu, Meng; Strawhecker, Kenneth E.; Shazly, Tarek; Edelman, Elazer; VanLandingham, Mark R.; Smith, James F.; Van Vliet, Krystyn J.

    2011-03-01

    For both materials engineering research and applied biomedicine, a growing need exists to quantify mechanical behaviour of tissues under defined hydration and loading conditions. In particular, characterisation under dynamic contact-loading conditions can enable quantitative predictions of deformation due to high rate 'impact' events typical of industrial accidents and ballistic insults. The impact indentation responses were examined of both hydrated tissues and candidate tissue surrogate materials. The goals of this work were to determine the mechanical response of fully hydrated soft tissues under defined dynamic loading conditions, and to identify design principles by which synthetic, air-stable polymers could mimic those responses. Soft tissues from two organs (liver and heart), a commercially available tissue surrogate gel (Perma-Gel™) and three styrenic block copolymer gels were investigated. Impact indentation enabled quantification of resistance to penetration and energy dissipative constants under the rates and energy densities of interest for tissue surrogate applications. These analyses indicated that the energy dissipation capacity under dynamic impact increased with increasing diblock concentration in the styrenic gels. Under the impact rates employed (2 mm/s to 20 mm/s, corresponding to approximate strain energy densities from 0.4 kJ/m3 to 20 kJ/m3), the energy dissipation capacities of fully hydrated soft tissues were ultimately well matched by a 50/50 triblock/diblock composition that is stable in ambient environments. More generally, the methodologies detailed here facilitate further optimisation of impact energy dissipation capacity of polymer-based tissue surrogate materials, either in air or in fluids.

  9. Thermo-physical properties of silica gel for adsorption desalination cycle

    KAUST Repository

    Thu, Kyaw

    2013-02-01

    Thermo-physical properties, surface characteristics and water vapor uptake capacity are key parameters in the selection of adsorbent for an adsorption desalination (AD) cycle. In the AD cycles, silica gel is used as adsorbent due to their high water vapor uptake capacity, reliability, repeatability and inexpensiveness as compared to other adsorbents. Three types of commercially available silica gels (Type-RD 2560,Type-A5BW and Type-A++) are investigated using a surface characteristic analyzer and their thermo-physical properties are evaluated using several analysis methods. The instrument used in this investigation employs the static volumetric method with liquid Nitrogen at 77 K as the filing fluid. The surface area of each adsorbent is studied using Brunauer-Emmett-Teller (BET) method whilst the pore size distribution (PSD) analysis is conducted with the Non-Local Density Functional Theory (NLDFT). It is observed that the Type-A++ silica gel (granular type) possesses the highest surface area of 863.6 m2/g amongst the three parent silica gels studied. It has a two-maxima or bimodal distribution pattern where the pore diameters are distributed mostly between 10 Å and 30 Å. Water vapor uptake capacity of silica gels are studied with water vapor dosage apparatus and the results show that the Type-A++ silica gel exhibits a highest equilibrium uptake at 537 cm3/g. These thermo-physical properties are essential for the design and the numerical simulation of AD cycles. © 2012 Published by Elsevier Ltd.

  10. Porous Silica Sol-Gel Glasses Containing Reactive V2O5 Groups

    Science.gov (United States)

    Stiegman, Albert E.

    1995-01-01

    Porous silica sol-gel glasses into which reactive vanadium oxide functional groups incorporated exhibit number of unique characteristics. Because they bind molecules of some species both reversibly and selectively, useful as chemical sensors or indicators or as scrubbers to remove toxic or hazardous contaminants. Materials also oxidize methane gas photochemically: suggests they're useful as catalysts for conversion of methane to alcohol and for oxidation of hydrocarbons in general. By incorporating various amounts of other metals into silica sol-gel glasses, possible to synthesize new materials with broad range of new characteristics.

  11. Organically Modified Aero-Sol Gel Silica for Elastomer Reinforcement

    Science.gov (United States)

    Pratsinis, S. E.; Kohls, D. J.; Beaucage, G.

    2000-03-01

    We have developed facilities to produce organically functionalized silicas using a novel, room-temperature, aerosol, chemical reactor (ASG reactor). This reactor can produce exceedingly high surface area nano-structured materials (up to 800 m2/g) with tuned interfacial chemistries. This poster will present our results on dynamic mechanical properties of elastomer compounds with ASG-organically modified silicas and comparison with conventional carbon black, conventional precipated and fumed silica as well as blends of the conventional materials. The mass-fractal structure as determined by SAXS and SALS, as well as conventional gas and DBP absorption measurements and microscopy will be presented. Hyeon-Lee, J.; Beaucage, G.; Pratsinis, S. E. (1997) Chem. of Mat. 9, 2400. Hyeon-Lee, J.; Beaucage, G.; Pratsinis, S. E.; Vemury, S. (1998) Langmuir 5751.

  12. Mixed Pyridine-phenol Boron Complex Encapsulated in Polymer/Silica Hybrid Sol-gel Matrix

    Institute of Scientific and Technical Information of China (English)

    DONG Wei; TANG Jun; WANG Yue

    2008-01-01

    A novel pyridine-phenol boron complex[(dppy)BF]was encapsulated into polymer/silica composite matrix by sol-gel process.UV-Vis absorption spectra show that this process can control the aggregation structure of complex(dppy)BF.The results of photoluminescence of(dppy)BF in sol-gel composite film indicate that both fluorescence intensity and photostability are markedly increased using this method compared with other methods,which increases the practical significance of such composite film.

  13. SOL-GEL SILICA-BASED Ag–Ca–P COATINGS WITH AGRESSIVE PRETREATMENT OF TITANIUM SUBSTRATE

    OpenAIRE

    2011-01-01

    The aim of the experiment was the obtaining of thin silica coatings on titanium by sol-gel method, using mechanical (SiC - paper No.180) and chemical (leaching in HF) pretreatments of the titanium substrates. The solutions were based on TEOS. For the sol-gel dipping process 4 different solutions were prepared: silica, silica with AgNO3 and silica + AgNO3 with brushite (CaHPO4·2H2O) or monetite (CaHPO4) powders. The solutions were aged for 7 and 14 days at laboratory temperature. After sol-gel...

  14. Stability of poly(vinylidene fluoride-co-hexafluoropropylene)-based composite gel electrolytes with functionalized silicas

    Energy Technology Data Exchange (ETDEWEB)

    Walkowiak, Mariusz [Central Laboratory of Batteries and Cells, Forteczna 12 St., 61-362 Poznan (Poland); Zalewska, Aldona [Warsaw University of Technology, Department of Chemistry, Noakowskiego 3 St., 00-664 Warsaw (Poland); Jesionowski, Teofil [Poznan University of Technology, Institute of Chemical Technology and Engineering, Marii Sklodowskiej-Curie 2 Sq., 60-965 Poznan (Poland); Pokora, Monika [Central Laboratory of Batteries and Cells, Forteczna 12 St., 61-362 Poznan (Poland); Poznan University of Technology, Institute of Chemical Technology and Engineering, Marii Sklodowskiej-Curie 2 Sq., 60-965 Poznan (Poland)

    2007-11-15

    Various aspects of stability of composite polymer gel electrolytes based on poly(vinylidene fluoride-co-hexafluoropropylene) (PVdF/HFP) polymeric matrix and functionalized precipitated silicas have been studied. The silica fillers have been surface modified with methacryloxy or vinyl groups by partially replacing silanol groups, so that bi-functional (hydrophilic/hydrophobic) character of the inorganic fillers was created. Compatibility of the gel electrolytes with lithium electrode has been examined by means of EIS technique. Electrochemical stability window has been studied with the application of cyclic voltammetry technique with fast sweeping rate. Passive layer formation on graphite electrode has been investigated for all the gel electrolytes by means of cyclic voltammetry with slow scan rate and galvanostatic charging/discharging technique. It has been shown that stability of the interface between lithium and gel electrolyte is significantly improved when bi-functional silicas are used as fillers. The phenomenon has been ascribed to more effective scavenging of trace impurities as well as to better shielding of the electrode surfaces. Cyclic voltammetry on platinum has revealed excessive electrochemical redox processes upon prolonged cycling for all the gel electrolytes. It has been demonstrated that stable passive layers are formed on graphite electrodes upon electrochemical reduction in the presence of the studied composite polymer gel electrolytes. (author)

  15. Studies on impact sensitivity of nanosized trinitrotoluene (TNT) confined in silica processed by sol-gel method

    Institute of Scientific and Technical Information of China (English)

    S.V. INGALE; P.B. WAGH; P.U. SASTRY; C.B. BASAK; D. BANDYOPADHYAY; S.B. PHAPALE; Satish C. GUPTA

    2016-01-01

    Nano-sized trinitrotoluene (TNT) material restrained in silica gel has been prepared by using the sol-gel process to study the effect of varying porosity in gel on the sensitivity of TNT. The TNT content in the gel has been varied from 60 to 90 wt%(at fixed acetone/tetramethoxysilane ratio of 50). Also, for a fixed TNT content of 75 wt%, the pore structure in the gel has been varied by changing the ratio of silica gel precursor to the solvent. The resultant TNT–silica gel composites have been characterized using scanning electron microscopy, thermal analysis, small angle X-ray scattering and surface area analysis techniques. Impact sensitivity studies were carried out using Fall Hammer Impact Test. The results showed that the sensitivity of nanostructured explosives prepared by sol-gel process can be tailored precisely by controlling the process parameters.

  16. Aplicação e modificação química da sílica gel obtida de areia Aplication and chemical modification of silica-gel obtained from sand

    OpenAIRE

    Prado,Alexandre G. S.; Faria,Elaine A.; Pedro M. Padilha

    2005-01-01

    The silica gel was obtained from sand and its surface was modified with POCl3 to produce Si-Cl bonds on the silica surface. Ethylenediamine was covalently bonded onto the chlorinated silica surface. The adsorption of the chlorides of divalent cobalt, nickel and copper was qualitatively studied to show that the bonding of ethylenediamine onto the silica gel surface produces a solid base capable of chelating metal ions from solution. The experiments illustrate the extraction of silica gel, its ...

  17. Mechanochemical and silica gel-mediated formation of highly electron-poor 1-cyanocarbonylferrocene.

    Science.gov (United States)

    Nieto, Daniel; Bruña, Sonia; Montero-Campillo, M Merced; Perles, Josefina; González-Vadillo, Ana Ma; Méndez, Julia; Mo, Otilia; Cuadrado, Isabel

    2013-10-28

    Simple manual grinding of solid cyanomethylferrrocene (1) and silica gel provides a facile one-pot access route to prepare unexpected and highly electron-poor metallocene, 1-cyanocarbonylferrocene (2). Electrochemical measurements supported by computational studies reveal that 2 exhibits the highest Fe(II)/Fe(III) oxidation potential reported for mono-substituted ferrocenes.

  18. Investigation of the processes of impregnation and drying of granular silica gel

    Science.gov (United States)

    Fedorov, A. V.; Zhilin, A. A.; Korobeinikov, Yu. G.

    2011-09-01

    The process of capillary impregnation and drying of silica gel grains in the acousto-convective drier of the ITPM of the Siberian branch of the Russian Academy of Sciences has been investigated experimentally. Two methods for humidifying a material with developed surface and internal structures have been considered. A comparison of these methods has been made and the influence of the impregnation rate on the geometry of silica gel grains has been analyzed. Silica gel grains were dried by three methods: microwave, convective, and acousto-convective. The dependence of the drying rate and the quality of the dried material on the chosen drying method has been shown. To describe the moisture extraction, we propose a mathematical model based on a two-dimensional diffusion equation written in the cylindrical system of coordinates. The moisture distribution in cylindrical samples consisting of silica gel grains has been obtained numerically for various values of the initial moisture content with the use of certain diffusion coefficients and the dependence of the moisture transfer coefficient on the frequency of acousto-convective action.

  19. Synthesis and Evaluation of Molecularly Imprinted Silica Gel for 2-Hydroxybenzoic Acid in Aqueous Solution

    Directory of Open Access Journals (Sweden)

    Mhd Radzi Abas

    2013-03-01

    Full Text Available A molecularly imprinted silica gel sorbent for selective removal of 2-Hydroxybenzoic acid (2-HA was prepared by a surface imprinting technique with a sol-gel process. The 2-HA molecularly imprinted silica gel (2-HA-MISG sorbent was evaluated by various parameters, including the influence of pH, static, kinetic adsorption and selectivity experiments. The optimum adsorption capacity to the 2-HA appeared to be around pH 2 by the polymer. Morevoer, the imprinted sorbent displayed fast uptake kinetics, obtained within 20 min. The adsorption capacity of the 2-HA-MISG (76.2 mg g−1 was higher than that of the non-imprinted silica gel (NISG (42.58 mg g−1. This indicates that the 2-HA-MISG offers a higher affinity for 2-HA than the NISG. The polymer displays good selectivity and exhibits good reusability. Experimental results show the potential of molecularly imprinted silica sorbent for selective removal of 2-HA.

  20. Thin-film silica sol-gels doped with ion responsive fluorescent lipid bilayers

    Energy Technology Data Exchange (ETDEWEB)

    Sasaki, D.Y.; Shea, L.E.; Sinclair, M.B.

    1999-01-12

    A metal ion sensitive, fluorescent lipid-b i layer material (5oA PSIDA/DSPC) was successfully immobilized in a silica matrix using a tetramethoxysilane (TMOS) sol-gel procedure. The sol-gel immobilization method was quantitative in the entrapment of seif-assembled Iipid-bilayers and yielded thin films for facile configuration to optical fiber piatforms. The silica matrix was compatible with the solvent sensitive lipid bilayers and provided physical stabilization as well as biological protection. Immobilization in the silica sol-gel produced an added benefit of improving the bilayer's metal ion sensitivity by up to two orders of magnitude. This enhanced performance was attributed to a preconcentrator effect from the anionic surface of the silica matrix. Thin gels (193 micron thickness) were coupled to a bifurcated fiber optic bundle to produce a metal ion sensor probe. Response times of 10 - 15 minutes to 0.1 M CUCIZ were realized with complete regeneration of the sensor using an ethylenediarninetetraacetic acid (EDTA) solution.

  1. The effect of silica-coating by sol-gel process on resin-zirconia bonding.

    Science.gov (United States)

    Lung, Christie Ying Kei; Kukk, Edwin; Matinlinna, Jukka Pekka

    2013-01-01

    The effect of silica-coating by sol-gel process on the bond strength of resin composite to zirconia was evaluated and compared against the sandblasting method. Four groups of zirconia samples were silica-coated by sol-gel process under varied reagent ratios of ethanol, water, ammonia and tetraethyl orthosilicate and for different deposition times. One control group of zirconia samples were treated with sandblasting. Within each of these five groups, one subgroup of samples was kept in dry storage while another subgroup was aged by thermocycling for 6,000 times. Besides shear bond testing, the surface topography and surface elemental composition of silica-coated zirconia samples were also examined using scanning electron microscopy and X-ray photoelectron spectroscopy. Comparison of silica coating methods revealed significant differences in bond strength among the Dry groups (psol-gel deposition times also revealed significant differences in bond strength among the Dry groups (pcoating of zirconia by sol-gel process resulted in weaker resin bonding than by sandblasting.

  2. Efficient CO2 capture on low-cost silica gel modified by polyethyleneimine

    Institute of Scientific and Technical Information of China (English)

    Ke Wang; Hongyan Shang; Lin Li; Xinlong Yan; Zifeng Yan; Chenguang Liu; Qingfang Zha

    2012-01-01

    In this work,a series of polyethyleneimine (PEI) functionalized commercial silica gel were prepared by wet impregnation method and used as CO2 sorbent.The as-prepared sorbents were characterized by N2 adsorption,FT-IR and SEM techniques.CO2 capture was tested in a fixed bed reactor using a simulated flue gas containing 15.1% CO2 in a temperature range of 25-100 ℃.The effects of sorption temperature and amine content on CO2 uptake of the adsorbents were investigated.The silica gel with a 30 wt% PEI loading manifested the largest CO2 uptake of 93.4 mgCO2/gadsorbent (equal to 311.3 mgCO2/gPEI) among the tested sorbents under the conditions of 15.1% (v/v) CO2 in N2 at 75 ℃ and atmospheric pressure.Moreover,it was rather low-cost.In addition,the PEI-impregnated silica gel exhibited stable adsorption-desorption behavior during 5 consecutive test cycles.These results suggest that the PEI-impregnated silica gel is a promising and cost-effective sorbent for CO2 capture from flue gas and other stationary sources with low CO2 concentration.

  3. Immobilization of Magnetic Nanoparticles onto Amine-Modified Nano-Silica Gel for Copper Ions Remediation

    Directory of Open Access Journals (Sweden)

    Marwa Elkady

    2016-06-01

    Full Text Available A novel nano-hybrid was synthesized through immobilization of amine-functionalized silica gel nanoparticles with nanomagnetite via a co-precipitation technique. The parameters, such as reagent concentrations, reaction temperature and time, were optimized to accomplish the nano-silica gel chelating matrix. The most proper amine-modified silica gel nanoparticles were immobilized with magnetic nanoparticles. The synthesized magnetic amine nano-silica gel (MANSG was established and characterized using X-ray diffraction (XRD, transmission electron microscopy (TEM, scanning electron microscopy (SEM, Fourier transform infrared (FTIR, thermal gravimetric analysis (TGA, differential scanning calorimetry (DSC and vibrating sample magnetometry (VSM. The feasibility of MANSG for copper ions’ remediation from wastewater was examined. MANSG achieves a 98% copper decontamination from polluted water within 90 min. Equilibrium sorption of copper ions onto MANSG nanoparticles obeyed the Langmuir equation compared to the Freundlich, Temkin, Elovich and Dubinin-Radushkevich (D-R equilibrium isotherm models. The pseudo-second-order rate kinetics is appropriate to describe the copper sorption process onto the fabricated MANSG.

  4. Synthesis and evaluation of molecularly imprinted silica gel for 2-hydroxybenzoic Acid in aqueous solution.

    Science.gov (United States)

    Raof, Siti Farhana Abdul; Mohamad, Sharifah; Abas, Mhd Radzi

    2013-03-14

    A molecularly imprinted silica gel sorbent for selective removal of 2-Hydroxybenzoic acid (2-HA) was prepared by a surface imprinting technique with a sol-gel process. The 2-HA molecularly imprinted silica gel (2-HA-MISG) sorbent was evaluated by various parameters, including the influence of pH, static, kinetic adsorption and selectivity experiments. The optimum adsorption capacity to the 2-HA appeared to be around pH 2 by the polymer. Morevoer, the imprinted sorbent displayed fast uptake kinetics, obtained within 20 min. The adsorption capacity of the 2-HA-MISG (76.2 mg g-1) was higher than that of the non-imprinted silica gel (NISG) (42.58 mg g-1). This indicates that the 2-HA-MISG offers a higher affinity for 2-HA than the NISG. The polymer displays good selectivity and exhibits good reusability. Experimental results show the potential of molecularly imprinted silica sorbent for selective removal of 2-HA.

  5. Sol-gel network silica/modified montmorillonite clay hybrid nanocomposites for hydrophobic surface coatings.

    Science.gov (United States)

    Meera, Kamal Mohamed Seeni; Sankar, Rajavelu Murali; Murali, Adhigan; Jaisankar, Sellamuthu N; Mandal, Asit Baran

    2012-02-01

    Sol-gel silica/nanoclay composites were prepared through sol-gel polymerization technique using tetraethylorthosilicate precursor and montmorillonite (MMT) clay in aqueous media. In this study, both montmorillonite-K(+) and organically modified MMT (OMMT) clays were used. The prepared composites were coated on glass substrate by making 1 wt% solution in ethyltrichlorosilane. The incorporation of nanoclay does not alter the intensity of characteristic Si-O-Si peak of silica network. Thermogravimetric studies show that increasing clay content increased the degradation temperature of the composites. Differential scanning calorimetry (DSC) results of organically modified MMT nanoclay incorporated composite show a shift in the melting behavior up to 38°C. From DSC thermograms, we observed that the ΔH value decreased with increasing clay loading. X-ray diffraction patterns prove the presence of nanoclay in the composite and increase in the concentration of organically modified nanoclay from 3 to 5 wt% increases the intensity of the peak at 2θ=8° corresponds to OMMT. Morphology of the control silica gel composite was greatly influenced by the incorporation of OMMT. The presence of nanoclay changed the surface of control silica gel composite into cleaved surface with brittle in nature. Contact angle measurements were done for the coatings to study their surface behavior. These hybrid coatings on glass substrate may have applications for hydrophobic coatings on leather substrate.

  6. Rheology of the gelation process of silica gel

    OpenAIRE

    Filho, O. K.; Aegerter, Michel A.

    1988-01-01

    The rheology of silica sols prepared from mixtures of tetramethoxysilane (TMOS)-methanol-water under basic neutral conditions has been studied at 25, 40 and 60 ° C during the gelation process. The sols show non-Newtonian pseudoplastic behavior from the time of preparation with the appearance of yield stress near the gelation point. The results are analysed using rheological equations of state and the concept of the point of gelation is discussed. For neutral sols an apparent activation energy...

  7. Microstructure Control of Nanoporous Silica Thin Film Prepared by Sol-gel Process

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Nanoporous silica films were prepared by sol-gel process with base, acid and base/acid two-step catalysis.Transmission electron microscope (TEM) and particle size analyzer were used to characterize the microstructure and the particle size distribution of the sols. Scanning electron microscopy (SEM), atomic force microscopy (AFM) and spectroscopic ellipsometer were used to characterize the surface microstructure and the optical properties of the silica films. Stability of the sols during long-term storage was investigated. Moreover,the dispersion relation of the optical constants of the silica films, and the control of the microstructure and properties of the films by changing the catalysis conditions during sol-gel process were also discussed.

  8. Spectroscopic studies of Cu2+ ions in sol–gel derived silica matrix

    Indian Academy of Sciences (India)

    P I Paulose; Gin Jose; Vinoy Thomas; Gijo Jose; N V Unnikrishnan; M K R Warrier

    2002-02-01

    The Cu2+ ion doped silica gel matrices in monolithic shape were prepared by hydrolysis and condensation of tetraethyl orthosilicate (TEOS). The absorption, transmittance and fluorescence spectra of the gel matrices heat treated at different temperatures were monitored. The loss of water and hydroxyl group from silica network changes the optical properties of the Cu2+ ions in the host, noted by the change in colour of monolith and spectral characteristics. The pronounced blue shift observed (700–900 nm to 600–850 nm) for the broad band of the absorption spectra of the samples heated up to 700°C is attributed to the ligand field splitting and partial removal of hydroxyl group from the silica matrices. The results indicate broadband filtering effects of the samples in the wavelength region 400–600 nm. Absorption and fluorescence spectra of the glass matrices heated to 1000°C confirms the conversion of Cu2+ ion to Cu+ ion.

  9. Mesoporous Silica Materials Synthesized via Sol-Gel Methods Modified with Ionic Liquid and Surfactant Molecules

    Institute of Scientific and Technical Information of China (English)

    Cun-ying Xu; Ru-lan Tang; Yi-xin Hu; Peng-xiang Zhang

    2008-01-01

    Mesoporous silica materials were synthesized via a sol-gel method employing a room temperature ionic liquid (1-butyl-3-methylimidazolium tetrafluoroborate, [bmim][BF4]) as a new solvent medium and further modified with surfactant (hexadecyl-trimethyl-ammonium bromide, CTAB) as a pore templating material. The synthesized samples were characterized by the transmission electron microscopy, X-ray diffraction, and N2 adsorption-desorption techniques. The results indicated that the mesoporous silica synthesized by using [bmim][BF4] and CTAB as mixed templates showed better mesostructural order and smaller pore size, compared with mesoporous silica materials synthesized by using single [bmim][BF4]as template under the same conditions. This indicates that the presence of surfactant can affect the microstructures of silica prepared by the present synthesis method.

  10. Probing the hydration of composite cement pastes containing fly ash and silica fume by proton NMR spin-lattice relaxation

    Institute of Scientific and Technical Information of China (English)

    2010-01-01

    Proton NMR spin-lattice relaxation (T1) was used as a prober for observing the hydration process of composite cement pastes blending fly ash and silica fume during the early age.The distribution at initial time,evolution curves and signals intensity of T1 were shown in this paper.Results demonstrate that the T1 distribution curves at initial time exhibit two peaks,which are regarded as two different water phases in the pastes.The evolution curves of T1 are in good agreement with the hydration process of composite pastes and could be roughly divided into four stages:initial period,dormant period,acceleration period and steady period.The hydration mechanism for each stage was discussed.The hydration of the composite cement pastes was retarded by the addition of fly ash and silica fume when compared to that of pure cement.However,the hydration degree of the cement in the blends was promoted.

  11. RESIDUAL TLC SILICA GEL: RECUPERATION PROCESS, CHARACTERIZATION AND APPLICATION.

    Directory of Open Access Journals (Sweden)

    Maria Alexsandra de Sousa Rios

    2017-06-01

    Full Text Available A utilização de sílica gel de forma intensiva em laboratórios químicos tem um custo elevado, e gera uma quantidade significativa de resíduos sólidos contaminados com compostos orgânicos. Nesse sentido, a busca de métodos eficazes para reduzir os impactos que este material pode causar ao meio ambiente, tem sido um fator de motivação para muitos pesquisadores, uma vez que a sua utilização tem crescido bastante no segmento de pesquisa científica. Assim, o presente trabalho apresenta o processo de recuperação, caracterização e aplicação do gel de sílica 60G, um adsorvente usado na preparação de Cromatografia de Camada Fina. De acordo com os resultados, o método proposto foi capaz de recuperar o gel de sílica residual, tornando-se possível, para ser reutilizado no processo de separação e/ou purificação de compostos orgânicos de um modo prático e com um impacto ambiental reduzido.

  12. Electrical conduction in composites containing copper core-copper oxide shell nanostructure in silica gel

    Indian Academy of Sciences (India)

    D Das; T K Kundu; M K Dey; S Chakraborty; D Chakravorty

    2003-10-01

    Composites of nanometre-sized copper core-copper oxide shell with diameters in the range 6.1 to 7.3 nm dispersed in a silica gel were synthesised by a technique comprising reduction followed by oxidation of a suitably chosen precursor gel. The hot pressed gel powders mixed with nanometre-sized copper particles dispersed in silica gel showed electrical resistivities several orders of magnitude lower than that of the precursor gel. Electrical resistivities of the different specimens were measured over the temperature range 30 to 300°C. Activation energies for the coreshell nanostructured composites were found to be a fraction of that of the precursor gel. Such dramatic changes are ascribed to the presence of an interfacial amorphous phase. The resistivity variation as a function of temperature was analysed on the basis of Mott’s small polaron hopping conduction model. The effective dielectric constant of the interfacial phase as extracted from the data analysis was found to be much higher than that of the precursor glass. This has been explained as arising from the generation of very high pressure at the interface due to the oxidation step to which the copper nanoparticles are subjected.

  13. SILICA GEL BEHAVIOR UNDER DIFFERENT EGS CHEMICAL AND THERMAL CONDITIONS: AN EXPERIMENTAL STUDY

    Energy Technology Data Exchange (ETDEWEB)

    Hunt, J D; Ezzedine, S M; Bourcier, W; Roberts, S

    2012-01-19

    Fractures and fracture networks are the principal pathways for migration of water and contaminants in groundwater systems, fluids in enhanced geothermal systems (EGS), oil and gas in petroleum reservoirs, carbon dioxide leakage from geological carbon sequestration, and radioactive and toxic industrial wastes from underground storage repositories. When dealing with EGS fracture networks, there are several major issues to consider, e.g., the minimization of hydraulic short circuits and losses of injected geothermal fluid to the surrounding formation, which in turn maximize heat extraction and economic production. Gel deployments to direct and control fluid flow have been extensively and successfully used in the oil industry for enhanced oil recovery. However, to the best of our knowledge, gels have not been applied to EGS to enhance heat extraction. In-situ gelling systems can either be organic or inorganic. Organic polymer gels are generally not thermostable to the typical temperatures of EGS systems. Inorganic gels, such as colloidal silica gels, however, may be ideal blocking agents for EGS systems if suitable gelation times can be achieved. In the current study, we explore colloidal silica gelation times and rheology as a function of SiO{sub 2} concentration, pH, salt concentration, and temperature, with preliminary results in the two-phase field above 100 C. Results at 25 C show that it may be possible to choose formulations that will gel in a reasonable and predictable amount of time at the temperatures of EGS systems.

  14. b-diketonates of Eu3+, red phosphors, supported on sol-gel functionalised silica

    Directory of Open Access Journals (Sweden)

    Nassar Eduardo J.

    2001-01-01

    Full Text Available Silica gel was functionalised with chloropropyl groups through the sol-gel process and then a beta-diketone was incorporated into the support. Afterwards, Eu3+ ion and its chelates of 1,10-phenantroline (phen and 2,2'-bipyridine (bpy, red phosphors, were supported on such silica. Luminescence studies of Eu3+ bound to this new material have shown that there is an increase in the intensity of the emission when the ion is isolated by ligands in the silica matrix. The energy transfer from the ligands phen and bpy to Eu3+ ion was observed in the excitation spectra, which present new bands ascribed to the ligands and/or complex. The Eu3+-functionalised silica was characterised by TGA and FTIR. TGA analysis showed that there is a large loss of mass around 300 °C, which is ascribed to the organic part of the material. The FTIR spectra presented the vibration modes for Si-C and -CH2-. The luminescent properties of the ions surrounding the Eu3+ ion were studied. The decay curve displayed a bi-exponential behaviour, indicating that there is more than one site of Eu3+ on the surface of the silica.

  15. Silica-Copper Oxide Composite Thin Films as Solar Selective Coatings Prepared by Dipping Sol Gel

    Directory of Open Access Journals (Sweden)

    E. Barrera-Calva

    2008-01-01

    Full Text Available Silica-copper oxide (silica-CuO composite thin films were prepared by a dipping sol-gel route using ethanolic solutions comprised TEOS and a copper-propionate complex. Sols with different TEOS/Cu-propionate (Si/Cu molar ratios were prepared and applied on stainless steel substrates using dipping process. During the annealing process, copper-propionate complexes developed into particulate polycrystalline CuO dispersed in a partially crystallized silica matrix, as indicated by the X-ray diffraction (XRD and X-ray photoelectron spectroscopy (XPS analyses. The gel thermal analysis revealed that the prepared material might be stable up to 400°C. The silica-CuO/stainless steel system was characterized as a selective absorber surface and its solar selectivity parameters, absorptance (α, and emittance (ε were evaluated from UV-NIR reflectance data. The solar parameters of such a system were mostly affected by the thickness and phase composition of the SiO2-CuO film. Interestingly, the best solar parameters (α = 0.92 and ε = 0.2 were associated to the thinnest films, which comprised a CuO-Cu2O mixture immersed in the silica matrix, as indicated by XPS.

  16. Evolution of microstructure in mixed niobia-hybrid silica thin films from sol-gel precursors.

    Science.gov (United States)

    Besselink, Rogier; Stawski, Tomasz M; Castricum, Hessel L; ten Elshof, Johan E

    2013-08-15

    The evolution of structure in sol-gel derived mixed bridged silsesquioxane-niobium alkoxide sols and drying thin films was monitored in situ by small-angle X-ray scattering. Since sol-gel condensation of metal alkoxides proceeds much faster than that of silicon alkoxides, the incorporation of d-block metal dopants into silica typically leads to formation of densely packed nano-sized metal oxide clusters that we refer as metal oxide building blocks in a silica-based matrix. SAXS was used to study the process of niobia building block formation while drying the sol as a thin film at 40-80°C. The SAXS curves of mixed niobia-hybrid silica sols were dominated by the electron density contrast between sol particles and surrounding solvent. As the solvent evaporated and the sol particles approached each other, a correlation peak emerged. Since TEM microscopy revealed the absence of mesopores, the correlation peak was caused by a heterogeneous system of electron-rich regions and electron poor regions. The regions were assigned to small clusters that are rich in niobium and which are dispersed in a matrix that mainly consisted of hybrid silica. The correlation peak was associated with the typical distances between the electron dense clusters and corresponded with distances in real space of 1-3 nm. A relationship between the prehydrolysis time of the silica precursor and the size of the niobia building blocks was observed. When 1,2-bis(triethoxysilyl)ethane was first hydrolyzed for 30 min before adding niobium penta-ethoxide, the niobia building blocks reached a radius of 0.4 nm. Simultaneous hydrolysis of the two precursors resulted in somewhat larger average building block radii of 0.5-0.6 nm. This study shows that acid-catalyzed sol-gel polymerization of mixed hybrid silica niobium alkoxides can be rationalized and optimized by monitoring the structural evolution using time-resolved SAXS.

  17. Difference of Mullite Whiskers between Ytterbia-Doped Aluminum Hydroxide-Silica Gel and Mechanochemical Process

    Institute of Scientific and Technical Information of China (English)

    2006-01-01

    A number of processing routes were developed for the synthesis of mullite whiskers. Mullite whiskers that were derived from ytterbia-doped aluminum hydroxide-silica gel were studied; another process for preparing mullite whiskers from Al2O3-SiO2 oxide mixtures by mechanochemical method was encountered by chance. The method of ytterbia-doped aluminum hydroxide-silica was used to enhance mullite formation from gel. For adding ytterbia, mullite formation can take place at 1000 ℃ and almost single-phase mullite can be achieved at 1150 ℃, which is a significantly lower temperature than mechanochemical method. This enhancement of mullite formation is also attributed to refinement of aluminum hydroxide-silica by gel. Furthermore, well-developed single-crystal mullite whiskers were produced from the gel powder instead of normal-shaped grains. The presence of YbO might have promoted the formation of nanosized Al2O3 particles, which then acted as a template leading to mullite whiskers at higher sintering temperature.

  18. Study of the release mechanism of Terminalia chebula extract from nanoporous silica gel.

    Science.gov (United States)

    Chakraborty, Suparna; Mitra, Manoj Kumar; Chaudhuri, Mahua Ghosh; Sa, Biswanath; Das, Satadal; Dey, Rajib

    2012-12-01

    Sol/gel-derived silica gel was prepared at room temperature from tetraethyl orthosilicate precursor. The extracts of Terminalia chebula (Haritoki) were entrapped into the porous silica gel. Fourier transform infrared analysis revealed the proper adsorption of herbal values in the nanopores of the silica gel. Porosity was estimated by transmission electron microscope studies. The release kinetics of the extract in both 0.1 N HCl, pH 1.2, and Phosphate-buffer saline (PBS), pH 7.2, were determined using UV-Vis spectroscopy. Different dissolution models were applied to release data in order to evaluate the release mechanisms and kinetics. Biphasic release patterns were found in every formulation for both the buffer systems. The kinetics followed a zero-order equation for first 4 h and a Higuchi expression in a subsequent timeline in the case of 0.1 N HCl. In the case of PBS, the formulations showed best linearity with a first-order equation followed by Higuchi's model. The sustained release of the extract predominantly followed diffusion and super case II transport mechanism. The release value was always above the minimum inhibitory concentration.

  19. Asymmetric bioreduction of acetophenones by Baker's yeast and its cell-free extract encapsulated in sol-gel silica materials

    Science.gov (United States)

    Kato, Katsuya; Nakamura, Hitomi; Nakanishi, Kazuma

    2014-02-01

    Baker's yeast (BY) encapsulated in silica materials was synthesized using a yeast cell suspension and its cell-free extract during a sol-gel reaction of tetramethoxysilane with nitric acid as a catalyst. The synthesized samples were fully characterized using various methods, such as scanning electron microscopy, nitrogen adsorption-desorption, Fourier transform infrared spectroscopy, thermogravimetry, and differential thermal analysis. The BY cells were easily encapsulated inside silica-gel networks, and the ratio of the cells in the silica gel was approximately 75 wt%, which indicated that a large volume of BY was trapped with a small amount of silica. The enzyme activity (asymmetric reduction of prochiral ketones) of BY and its cell-free extract encapsulated in silica gel was investigated in detail. The activities and enantioselectivities of free and encapsulated BY were similar to those of acetophenone and its fluorine derivatives, which indicated that the conformation structure of BY enzymes inside silica-gel networks did not change. In addition, the encapsulated BY exhibited considerably better solvent (methanol) stability and recyclability compared to free BY solution. We expect that the development of BY encapsulated in sol-gel silica materials will significantly impact the industrial-scale advancement of high-efficiency and low-cost biocatalysts for the synthesis of valuable chiral alcohols.

  20. Growth and Characterizations of Pure and Calcium Doped Cadmium Tartrate Crystals by Silica Gel Method

    Directory of Open Access Journals (Sweden)

    N. S. Patil

    2014-10-01

    Full Text Available In the present course of investigation, pure and calcium doped cadmium tartrate crystals were grown in silica gel at room temperature. The optimum conditions were obtained by varying various parameters such as pH of gel, concentration of gel, gel setting time, concentration of reactants etc. Crystals having different morphologies were obtained such as whitish semitransparent, star shaped, needle shaped. Especially, effect of doping of calcium into cadmium tartrate has been studied with respect of size and transparency. It is found that doping enhances the size and transparency of the crystals. As-grown crystals were characterized using scanning electronic microscope (SEM, UV, Energy dispersive X-ray spectroscopy (EDAX.

  1. Synthesis of mesoporous silica nanoparticles by sol–gel as nanocontainer for future drug delivery applications

    Energy Technology Data Exchange (ETDEWEB)

    Vazquez, N.I.; Gonzalez, Z.; Ferrari, B.; Castro, Y.

    2017-07-01

    Development of mesoporous silica nanoparticles as carriers for drug delivery systems has increased exponentially during the last decade. The present work is focused on the synthesis of silica carriers by sol–gel from tetraethyl orthosilicate (TEOS) as precursor of silica and cetyltrimethylammonium bromide (CTAB) as pore generating agent. The synthesis conditions were modified varying the molar ratio of water/TEOS, NH3/TEOS and amount of CTAB. The silica particles were characterized by scan electron microscopy techniques (FESEM), high resolution transmission electron microscopy (HR-TEM), N2 adsorption–desorption isotherms, Zeta-potential and Dynamic Light Scattering (DLS). The results show that the specific surface area and the porosity of silica particles were strongly affected by the addition of CTAB and the amount of H2O. The dispersion and stability of silica mesoporous particles is achieved in spite of the high surface reactivity. The synthesis formulation affects considerably to the particle morphology, which changes from spheres to rods when the molar ratio of H2O increases. A maximum specific surface area of 1480m2/g was obtained with pore sizes ranging 2.5–2.8nm. (Author)

  2. Facile and Controlled Synthesis of Silica Sol Nanospheres Through a Modified Sol-Gel Process

    Institute of Scientific and Technical Information of China (English)

    LI Jie; CHEN Lianxi; ZHANG Zhongming; JIAO Caibin

    2014-01-01

    An effective and reproducible preparation of silica sol nanospheres via a modified sol-gel process has been described. Monodisperse and stable silica sol nanospheres with uniformsize were successfully obtained through the optimized synthesis in which the mixture of tetraethyl orthosilicate (TEOS) and ethanol was followed by the addition of water and ammonium hydroxide (NH3) separately, and the size of silica sol spheres was strictly controlled in the range of 25-119 nm with a narrow size distribution by fine adjustment of several reaction parameters. Results showed that in the presence of low concentration of TEOS, spheres size rose first and reached maximum when H2O concentration was up to 66 g/L. However, the diameter of silica sol spheres decreased above 66 g/L of H2O concentration. Furthermore, it was also found that the size and size distribution of silica sol nanospheres were affected by NH3 concentration. As NH3 concentration increased from 15 to 35 g/L, the diameter declined from 83 to 64 nm. Nevertheless, higher NH3 concentration would result in relatively broad size distribution, and gelation occurred when NH3 concentration reached 44 g/L. In addition, the effect of the different feed rates of NH3 on the size growth of silica sol nanospheres was also discussed.

  3. Imprinted functionalized silica sol-gel for solid-phase extraction of triazolamin.

    Science.gov (United States)

    Jin, Guoyou; Zhang, Baofei; Tang, Youwen; Zuo, Xiongjun; Wang, Songcai; Tang, Jingyi

    2011-05-15

    A triazolam-imprinted silica microsphere was prepared by combining a surface molecular-imprinting technique with the sol-gel process. The results illustrate that the triazolam-imprinted silica microspheres provided using γ-aminopropyltriethoxysilane and phenyltrimethoxysilane as monomers exhibited higher selectivity than those provided from γ-aminopropyltriethoxysilane and methyltriethoxysilane. In addition, the optimum affinity occurred when the molar ratio of γ-aminopropyltriethoxysilane, phenyltrimethoxysilane, and the template molecule was 4.2:4.7:0.6. Retention factor (k) and imprinting factor (IF) of triazolam on the imprinted and non-imprinted silica microsphere columns were characterized using high performance liquid chromatography (HPLC) with different mobile phases including methanol, acetonitrile, and water solutions. The molecular selectivity of the imprinted silica microspheres was also evaluated for triazolam and its analogue compounds in various mobile phases. The better results indicated that k and IF of triazolam on the imprinted silica microsphere column were 2.1 and 35, respectively, when using methanol/water (1/1, v/v) as the mobile phase. Finally, the imprinted silica was applied as a sorbent in solid-phase extraction (SPE), to selectively extract triazolam and its metabolite, α-hydroxytriazolam, from human urine samples. The limits of detection (LOD) for triazolam and α-hydroxytriazolam in urine samples were 30 ± 0.21 ng mL(-1) and 33 ± 0.26 ng mL(-1), respectively.

  4. Synthesis of biocompatible hydrophobic silica-gelatin nano-hybrid by sol-gel process.

    Science.gov (United States)

    Smitha, S; Shajesh, P; Mukundan, P; Nair, T D R; Warrier, K G K

    2007-03-15

    Silica-biopolymer hybrid has been synthesised using colloidal silica as the precursor for silica and gelatin as the biopolymer counterpart. The surface modification of the hybrid material has been done with methyltrimethoxysilane leading to the formation of biocompatible hydrophobic silica-gelatin hybrid. Here we are reporting hydrophobic silica-gelatin hybrid and coating precursor for the first time. The hybrid gel has been evaluated for chemical modification, thermal degradation, hydrophobicity, particle size, transparency under the UV-visible region and morphology. FTIR spectroscopy has been used to verify the presence of CH(3) groups which introduce hydrophobicity to the SiO2-MTMS-gelatin hybrids. The hydrophobic property has also been tailored by varying the concentration of methyltrimethoxysilane. Contact angle by Wilhelmy plate method of transparent hydrophobic silica-gelatin coatings has been found to be as high as approximately 95 degrees . Oxidation of the organic group which induces the hydrophobic character occurs at 530 degrees C which indicates that the surface hydrophobicity is retained up to that temperature. Optical transmittance of SiO2-MTMS-gelatin hybrid coatings on glass substrates has been found to be close to 100% which will enable the hybrid for possible optical applications and also for preparation of transparent biocompatible hydrophobic coatings on biological substrates such as leather.

  5. Probing the interplay between factors determining reaction rates on silica gel using termolecular systems.

    Science.gov (United States)

    Kirkpatrick, Iain; Worrall, David R; Williams, Siân L; Buck, Craig J T; Meseguer, Rafael G

    2012-10-01

    In this study we have compared energy and electron transfer reactions in termolecular systems using a nanosecond diffuse reflectance laser flash photolysis technique. We have previously investigated these processes on silica gel surfaces for bimolecular systems and electron transfer in termolecular systems. The latter systems involved electron transfer between three arene molecules with azulene acting as a molecular shuttle. In this study we present an alternative electron transfer system using trans β-carotene as an electron donor in order to effectively immobilise all species except the shuttle, providing the first unambiguous evidence for radical ion mobility. In the energy transfer system we use naphthalene, a structural isomer of azulene, as the shuttle, facilitating energy transfer from a selectively excited benzophenone sensitiser to 9-cyanoanthracene. Bimolecular rate constants for all of these processes have been measured and new insights into the factors determining the rates of these reactions on silica gel have been obtained.

  6. Immobilized silver nanoparticles on silica gel as an efficient catalyst in nitroarene reduction

    Institute of Scientific and Technical Information of China (English)

    Ali Reza Kiasat; Roya Mirzajani; Fakhri Ataeian; Mehdi Fallah-Mehrjardi

    2010-01-01

    Nanoparticles have properties that can be fine-tuned by their size as well as shape.Hence,there is significant current interest in preparing nano-materials of small size dispersity and to arrange them in close-packed aggregates.This letter describes a way of synthesising silver nanoparticles and their protection to aggregate by silica gel.The combination of catalytic quantities of immobilized silver nanoparticles with reductive ability of NaBH4 efficiently reduces aromatic nitroarenes to the corresponding amines in aqueous medium.Noteworthy is that highly chemoselective reactions were achieved in the presence of other functional groups such as halogen and carboxylic acid groups.The silver particles immobilized on silica gel are stable in the presence of oxygen for several months.

  7. Recovery of DNA from Agarose Gel with Home-made Silica Milk

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    An usefulness of silica milk made with waste ultraviolet light tube for recovery of DNA fragment from agarose gel was represented. The glass milk is a water suspension of 50% fine silica powder prepared by grinding the crushed waste ultraviolet light tube with a porcelain mortar.It was showed that one microliter of the glass milk could bind more than 1 μg of DNA fragment,and DNA fragment in length from 125 bp to 23 kb could be efficiently recovered from agarose gel. The bound DNA could be eluted from the particle of SiO2 in the glass milk with a yield of about 60%-80%.The eluted DNA could be used in all manipulations in molecular cloning.

  8. The effect of glycine on the growth of calcium carbonate in alkaline silica gel

    Science.gov (United States)

    Gan, Xiong; He, Kunhuan; Qian, Baosong; Deng, Qin; Lu, Laixian; Wang, Yun

    2017-01-01

    Calcium carbonate was crystallized in alkaline silica gel with the presence of glycine. The crystallization proceeded with a counterdiffusion method by the reaction of calcium chloride and sodium carbonate. Optical microscopy observation showed a significant effect of glycine on the morphology control of calcite crystals. When the initial concentration of glycine was high enough (10 mg/mL, 20 mg/mL), spherical vaterite particles formed in alkaline silica gel concomitantly together with dumbbell shaped calcite particles. The in situ study by micro-Raman spectroscopy demonstrated that both vaterite and the concomitant calcite were stable phases during their growth processes since the initial appearance. A possible mechanism has been discussed to emphasize the effect of glycine on the nucleation of vaterite and the morphological control of calcite.

  9. Synthesis of Hydroxypropyl-β-cyclodextrin Bonded Silica-gel and its Application to Resolution

    Institute of Scientific and Technical Information of China (English)

    Jin Gang YU; Ke Long HUANG; Du Shu HUANG; Jin Yue PU

    2006-01-01

    In order to set up a simple and effective method for resolution of optical isomers,hydroxypropyl-β-cyclodextrin was bonded to silica-gel, which can be used for preparation of thin-layer chromatography plates. Resolution of clenbuterol and propranolol were investigated on these thin-layer chromatography plates using different combinations of solvent systems at ambient temperature. The best simultaneous resolution was achieved in solvent system of acetonitrilen-butanol (50:50, v/v). Rst values of resolution of clenbuterol hydrochloride and propranolol hydrochloride are 3.6 and 4.3, respectively. The spots of different enantiomers are separated clearly. The results showed that hydroxypropyl-β-cyclodextrin bonded silica-gel could be successful in resolution of chiral adrenergic drugs. The study offers a direct, rapid and reliable method for separation of this kind of optically active compounds.

  10. Hydration effects on the molecular structure of silica-supported vanadium oxide catalysts: A combined IR, Raman, UV–vis and EXAFS study

    NARCIS (Netherlands)

    Keller, D.E.; Visser, T.; Soulimani, F.; Koningsberger, D.C.; Weckhuysen, B.M.

    2007-01-01

    The effect of hydration on the molecular structure of silica-supported vanadium oxide catalysts with loadings of 1–16 wt.% V has been systematically investigated by infrared, Raman, UV–vis and EXAFS spectroscopy. IR and Raman spectra recorded during hydration revealed the formation of V–OH groups, c

  11. In situ generated silica in natural rubber latex via the sol–gel technique and properties of the silica rubber composites

    Energy Technology Data Exchange (ETDEWEB)

    Poompradub, Sirilux, E-mail: sirilux.p@chula.ac.th [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, 254 Phayathai Road, Bangkok 10330 (Thailand); Thirakulrati, Mantana [Program in Petrochemistry and Polymer Science, Faculty of Science, Chulalongkorn University, 254 Phayathai Road, Bangkok 10330 (Thailand); Prasassarakich, Pattarapan [Department of Chemical Technology, Faculty of Science, Chulalongkorn University, 254 Phayathai Road, Bangkok 10330 (Thailand)

    2014-03-01

    Natural rubber (NR) composites reinforced by silica generated in situ within the NR matrix were prepared by the sol–gel process using tetraethoxysilane (TEOS) as the silica precursor. The effect of the TEOS content, water: TEOS mole ratio, reaction time and temperature on the in situ silica content formed in the NR latex were investigated. The results indicated that the suitable condition to produce a high silica content (54 parts by weight per hundred parts of rubber (phr)) in the rubbery matrix was the use of 200 phr TEOS and a water: TEOS mole ratio of 28.9:1 at room temperature for 24 h. The curing, mechanical, and thermal properties of the composite materials were also investigated. Increasing the in situ silica content increased the cure time and improved the mechanical properties of the composite. Compared to the NR vulcanizates filled with the commercial (ex situ formed) silica, the mechanical and thermal properties of the in situ silica composite material were significantly improved. Transmission electron microscopy revealed that the in situ formed silica particles were well distributed within the NR matrix, in contrast to the clumping of the ex situ formed commercial silica within the NR matrix. - Highlights: • High in situ silica content in NR latex was obtained up to 54 phr. • A good dispersion of in situ silica filling into the rubbery matrix. • Comparison of silica generated in the rubber matrix using solid, solution and latex NR substrates. • A good reinforcement effect of in situ silica was observed on the NR vulcanizate. • Sol–gel method is an alternative way to develop a novel composite material.

  12. Tailoring the oxidation state of cobalt through halide functionality in sol-gel silica

    Science.gov (United States)

    Olguin, Gianni; Yacou, Christelle; Smart, Simon; Diniz da Costa, João C.

    2013-01-01

    The functionality or oxidation state of cobalt within a silica matrix can be tailored through the use of cationic surfactants and their halide counter ions during the sol-gel synthesis. Simply by adding surfactant we could significantly increase the amount of cobalt existing as Co3O4 within the silica from 44% to 77%, without varying the cobalt precursor concentration. However, once the surfactant to cobalt ratio exceeded 1, further addition resulted in an inhibitory mechanism whereby the altered pyrolysis of the surfactant decreased Co3O4 production. These findings have significant implications for the production of cobalt/silica composites where maximizing the functional Co3O4 phase remains the goal for a broad range of catalytic, sensing and materials applications. PMID:24022785

  13. Sol-Gel Synthesis of Ordered β-Cyclodextrin-Containing Silicas

    OpenAIRE

    Trofymchuk, Iryna Mykolaivna; Roik, Nadiia; Belyakova, Lyudmila

    2016-01-01

    New approaches for β-cyclodextrin-containing silicas synthesis were demonstrated. Materials with hexagonally ordered mesoporous structure were prepared by postsynthesis grafting and by co-condensation methods. β-Cyclodextrin activated by a N,N′-carbonyldiimidazole was employed for postsynthesis treatment of 3-aminopropyl-modified MCM-41 support as well as for sol-gel synthesis with β-cyclodextrin-containing organosilane and tetraethyl orthosilicate participation in the presence of cetyltrimet...

  14. [Adsorption and desorption of organic solvent vapours using silica gel (author's transl)].

    Science.gov (United States)

    Takata, T; Aoki, B

    1981-01-01

    For a simple analysis of organic solvent vapours in working environmental air, we investigated the following method. First, join the adsorption tube (2 ml of 60--80 mesh silica gel packed in a 5 mm phi x 18 cm glass tube) to hand vacuum pump and suck 200 ml of the sample air. After adsorption, join this adsorption tube to the sampling bottle under reduced pressure. Second, open the cock of the sampling bottle and heat only the adsorption tube in an oven for 3 min. In the operation mentioned above, organic solvent vapours desorbed from the silica gel transfer smoothly into the sampling bottle. After desorption, take 1 ml of air from the sampling bottle and determine the sample quantities with the gas chromatograph. Sample solvents used were as follows: n-hexane, cyclohexane, benzene, toluene, m-xylene, styrene, 1.1.1-trichloroethane, dichloromethane, tetrachloroethylene, ethylacetate, acetone, methyl-ethylketone, methylisobutylketone, methanol, ethanol, n-propanol, and n-butanol. We obtained the following results. (1) 60--80 mesh silica gel is appropriate for this method. (2) Heating temperature to get 100% recovery varies with the type of organic solvent. m-Xylene and styrene require 250 degrees C, methylisobutylketone and n-butanol 200 degrees C, and the others 150 degrees C. (3) If the adsorption tube is preserved in a freezer at -20 degrees C, no decrease is observed for up to 7 days. At room temperatures, however, 1.1.1-trichloroethane, dichloromethane, tetrachloroethylene, n-hexane, and cyclohexane decreased by the amount 4-10% in the tube for each 24-hour period. These sample should be preserved at lower temperatures soon after absorbing on the silica gel. This method is simple and accurate, so valid for analysis of organic solvent vapours in the working environmental air.

  15. Sol-Gel Processing of Low Dielectric Constant Nanoporous Silica Thin Films

    Science.gov (United States)

    2001-11-01

    under the influence of attractive van der Waals forces. Spin coating has been used to deposit the porous thin silica films on desired substrates. This...for spin coating using a Model PC 101 spinner by Headway Research, Inc. All the wafers were used as-received without any pretreatment process... spin coating . Spin coating did not start until the solution reached the about-to-gel point, approximately 6/7 of its gelation time. After spin

  16. High order operation of distributed feedback dye-doped sol-gel silica laser

    Institute of Scientific and Technical Information of China (English)

    Xiaolei Zhu(朱小磊); Dennis Lo(罗荫权)

    2003-01-01

    High order Bragg scattering (M = 2 and M = 3) operations of the distributed feedback dye dopedsol-gel silica lasers are achieved using the second harmonic output of a Nd:YAG laser as the pump. Laserlinewidth of less than 0.06 nm and conversion efficiency of 0.7% for M = 3 and 11% for M = 2 aremeasured. Wavelength tuning of about 15 nm around the emission center has been realized by varyingthe intersection angle.

  17. Augmentation of Cooling Output by Silica Gel-Water Adsorption Cycle Utilizing the Waste Heat of GHP

    Science.gov (United States)

    Homma, Hiroki; Araki, Nobuyuki

    The GHP (Gas engine Heat Pump) system is expected to have high energy-efficiency in utilizing the waste heat exhausted from a gas engine. In summer season, a silica gel-water adsorption cooling unit driven by the exhaust heat is considered as a cooling system for saving energy. In this work, an attempt was made to improve the COP of a silica gel-water adsorption cooling system by enhancing heat and mass transfer in the silica gel adsorption layer. A unit cell was introduced as a simplified model of adsorber for analyzing the phenomena of heat and mass transfer in the adsorbent. This cell was composed of a single tube with a silica gel layer bonded on its external surface. Optimization of heat and mass transfer characteristics for the unit cell was carried out by experimental and analytical approach.

  18. The Mechanism of Pseudomorphic Transformation of Spherical Silica Gel into MCM-41 Studied by PFG NMR Diffusometry

    National Research Council Canada - National Science Library

    Wolf-Dietrich Einicke; Dirk Enke; Muslim Dvoyashkin; Rustem Valiullin; Roger Gläser

    2013-01-01

      The pseudomorphic transformation of spherical silica gel (LiChrospher® Si 60) into MCM-41 was achieved by treatment at 383 K for 24 h with an aqueous solution of cetyltrimethylammonium hydroxide (CTAOH...

  19. Effectiveness of silica based sol-gel microencapsulation method for odorants and flavors leading to sustainable environment

    National Research Council Canada - National Science Library

    Ashraf, Muhammad Aqeel; Khan, Aysha Masood; Ahmad, Mushtaq; Sarfraz, Maliha

    2015-01-01

    .... The sol-gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties...

  20. Development of novel biocompatible hybrid nanocomposites based on polyurethane-silica prepared by sol gel process.

    Science.gov (United States)

    Rashti, Ali; Yahyaei, Hossein; Firoozi, Saman; Ramezani, Sara; Rahiminejad, Ali; Karimi, Roya; Farzaneh, Khadijeh; Mohseni, Mohsen; Ghanbari, Hossein

    2016-12-01

    Due to high biocompatibility, polyurethane has found many applications, particularly in development of biomedical devices. A new nanocomposite based on thermoset polyurethane and silica nanoparticles was synthesized using sol-gel method. Sol-gel process was fulfilled in two acidic and basic conditions by using tetraethylorthosilicate (TEOS) and trimethoxyisocyanatesilane as precursors. The hybrid films characterized for mechanical and surface properties using tensile strength, contact angle, ATR-FTIR and scanning electron microscopy. Biocompatibility and cytotoxicity of the hybrids were assessed using standard MTT, LDH and TUNEL assays. The results revealed that incorporation of silica nanoparticles was significantly improved tensile strength and mechanical properties of the hybrids. Based on the contact angle results, silica nanoparticles increased hydrophilicity of the hybrids. Biocompatibility by using human lung epithelial cell line (MRC-5) demonstrated that the hybrids were significantly less cytotoxic compared to pristine polymer as tested by MTT and LDH assays. TUNEL assay revealed no signs of apoptosis in all tested samples. The results of this study demonstrated that incorporation of silica nanoparticles into polyurethane lead to the enhancement of biocompatibility, indicating that these hybrids could potentially be used in biomedical field in particular as a new coating for medical implants.

  1. Hexavalent chromium removal from wastewater using aniline formaldehyde condensate coated silica gel.

    Science.gov (United States)

    Kumar, P Albino; Ray, Manabendra; Chakraborty, Saswati

    2007-05-08

    A resinous polymer, aniline formaldehyde condensate (AFC) coated on silica gel was used as an adsorbent in batch system for removal of hexavalent chromium from aqueous solution by considering the effects of various parameters like reaction pH, dose of AFC coated silica gel, initial Cr(VI) concentration and aniline to formaldehyde ratio in AFC synthesis. The optimum pH for total chromium [Cr(VI) and Cr(III)] adsorption was observed as 3. Total chromium adsorption was second order and equilibrium was achieved within 90-120 min. Aniline to formaldehyde ratio of 1.6:1 during AFC synthesis was ideal for chromium removal. Total chromium adsorption followed Freundlich's isotherm with adsorption capacity of 65 mg/g at initial Cr(VI) 200mg/L. Total chromium removal was explained as combinations of electrostatic attraction of acid chromate ion by protonated AFC, reduction of Cr(VI) to Cr(III) and bond formation of Cr(III) with nitrogen atom of AFC. Almost 40-84% of adsorbed chromium was recovered during desorption by NaOH, EDTA and mineral acids. AFC coated silica gel can be effectively used for treatment of chromium containing wastewaters as an alternative.

  2. Immobilization of Beauveria bassiana Lipase on Silica Gel by Physical Adsorption

    Directory of Open Access Journals (Sweden)

    Vanessa Hitomi Sugahara

    2014-12-01

    Full Text Available Extracellular lipase from Beauveria bassianastrain CG481 was immobilized by using thirteen different immobilization protocols. Silica gel was chosen as the most suitable adsorbent with 94.8% of activity yield. The adsorption on silica gel did not change the optimum pH (8.5 and temperature (45ºC values of the free lipase (FL for lipolytic activity, and it showed higher activities in extreme conditions (pH 9.0 to 10.5, 60ºC. The lipase immobilized on silica gel (ILS showed enhanced stability at pH 7.0 after 120 h incubation (69.0% when compared to FL (33.3%. The thermal stability was also enhanced by immobilization at 60ºC in aqueous (64.6% and organic medium (95.1%, while FL showed only 40.6% of residual activity in aqueous medium and exhibited no activity for esterification reaction in n-heptane. The treatment of ILS with 0.8 M NaCl prevented lipase desorption while Triton X-100 (0.1% resulted the enzyme leakage. The ILS was reused for four times for esterification reaction with 80.8% of initial activity.

  3. Preparation and Application Situation of Silica Gel%硅胶的制备及应用现状

    Institute of Scientific and Technical Information of China (English)

    赵希鹏

    2011-01-01

    硅胶不溶于水和任何溶剂,无毒无味,化学性质稳定,除强碱、氢氟酸外不与任何物质发生反应。根据其孔径的大小分为:大孔硅胶、粗孔硅胶、B型硅胶、细孔硅胶。由于孔隙结构的不同,因此它们的吸附性能各有特点。硅胶是一种高活性的吸附材料,通常以硅酸钠和硫酸为原料制备,文中介绍了各种硅胶的生产工艺,论述了硅胶的应用现状。%Silica gel was insoluble in water and any solvent,non-toxic and odorless,chemical stability,except strong alkali and hydrofluoric acid,and it can't react with any material.According to its aperture size's,it was divided into big pore silica gel,thick pore silica gel,the type B silica gel and the fine pore silica gel.Because the pore structure was different,so they had different features of adsorption performance.Silica gel was a highly active adsorption materials,usually prepared by the sodium silicate and sulfuric acid as raw material.Various silica gel production technology was introduced,and the present situation of the application of the silica gel was discussed.

  4. Incorporation of Mesoporous Silica Particles in Gelatine Gels: Effect of Particle Type and Surface Modification on Physical Properties

    NARCIS (Netherlands)

    Perez-Esteve, E.; Oliver, L.; Garcia, L.; Nieuwland, M.; Jongh, de H.H.J.; Martinez-Manez, R.; Barat, J.M.

    2014-01-01

    The aim of this work was to investigate the impact of mesoporous silica particles (MSPs) on the physicochemical properties of filled protein gels. We have studied the effect of the addition of different mesoporous silica particles, either bare or functionalized with amines or carboxylates, on the ph

  5. Incorporation of mesoporous silica particles in gelatine gels: Effect of particle type and surface modification on physical properties

    NARCIS (Netherlands)

    Pérez-Esteve, E.; Oliver, L.; García, L.; Nieuwland, M.; Jongh, H.H.J. de; Martínez-Máñez, R.; Barat, J.M.

    2014-01-01

    The aim of this work was to investigate the impact of mesoporous silica particles (MSPs) on the physicochemical properties of filled protein gels. We have studied the effect of the addition of different mesoporous silica particles, either bare or functionalized with amines or carboxylates, on the ph

  6. Sol-gel preparation of silica and titania thin films

    Science.gov (United States)

    Thoř, Tomáš; Václavík, Jan

    2016-11-01

    Thin films of silicon dioxide (SiO2) and titanium dioxide (TiO2) for application in precision optics prepared via the solgel route are being investigated in this paper. The sol-gel process presents a low cost approach, which is capable of tailoring thin films of various materials in optical grade quality. Both SiO2 and TiO2 are materials well known for their application in the field of anti-reflective and also highly reflective optical coatings. For precision optics purposes, thickness control and high quality of such coatings are of utmost importance. In this work, thin films were deposited on microscope glass slides substrates using the dip-coating technique from a solution based on alkoxide precursors of tetraethyl orthosilicate (TEOS) and titanium isopropoxide (TIP) for SiO2 and TiO2, respectively. As-deposited films were studied using spectroscopic ellipsometry to determine their thickness and refractive index. Using a semi-empirical equation, a relationship between the coating speed and the heat-treated film thickness was described for both SiO2 and TiO2 thin films. This allows us to control the final heat-treated thin film thickness by simply adjusting the coating speed. Furthermore, films' surface was studied using the white-light interferometry. As-prepared films exhibited low surface roughness with the area roughness parameter Sq being on average of 0.799 nm and 0.33 nm for SiO2 and TiO2, respectively.

  7. Synthesis of palladium-doped silica nanofibers by sol-gel reaction and electrospinning process

    Energy Technology Data Exchange (ETDEWEB)

    San, Thiam Hui; Daud, Wan Ramli Wan; Kadhum, Abdul Amir Hassan; Mohamad, Abu Bakar; Kamarudin, Siti Kartom; Shyuan, Loh Kee; Majlan, Edy Herianto [Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia and Department of Chemical and Process Engineering, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia)

    2012-06-29

    Nanofiber is drawing great attention nowadays with their high surface area per volume and flexibility in surface functionalities that make them favorable as a proton exchange membrane in fuel cell application. In this study, incorporation of palladium nanoparticles in silica nanofibers was prepared by combination of a tetraorthosilane (TEOS) sol-gel reaction with electrospinning process. This method can prevent the nanoparticles from aggregation by direct mixing of palladium nanoparticles in silica sol. The as-produced electrospun fibers were thermally treated to remove poly(vinyl pyrrolidone) (PVP) and condensation of silanol in silica framework. PVP is chosen as fiber shaping agent because of its insulting and capping properties for various metal nanoparticles. Scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and Fourier transform infrared spectroscopy (FTIR) were used to characterize the silica fibers and Pd nanoparticles on the fibers. Spun fibers with average diameter ranged from 100nm to 400nm were obtained at optimum operating condition and distribution of Pd nanoparticles on silica fibers was investigated.

  8. Incorporation of Vanadium Oxide in Silica Nanofiber Mats via Electrospinning and Sol-Gel Synthesis

    Directory of Open Access Journals (Sweden)

    Jeanne E. Panels

    2006-01-01

    Full Text Available Submicron scale vanadia/silica hybrid nanofiber mats have been produced by electrospinning silica sol-gel precursor containing vanadium oxytriisopropoxide (VOTIP, followed by calcinations at high temperature. The properties of the resulting inorganic hybrid nanofiber mats are compared to those of electrospun pure silica nanofibers. SEM images show fibers are submicron in diameter and their morphology is maintained after calcination. Physisorption experiments reveal that silica nanofiber mats have a high specific surface area of 63 m2/g. FT-IR spectra exhibit Si—O vibrations and indicate the presence of V2O5 in the fibers. XPS studies reveal that the ratio of Si to O is close to 0.5 on the surface of fibers and the amount of vanadium on the surface of fibers increases with calcination. XRD diffraction patterns show that silica nanofibers are amorphous and orthorhombic V2O5 crystals have formed after calcination. EFTEM images demonstrate the growth of crystals on the surface of fibers containing vanadium after calcination. SEM images of fibers with high-vanadium content (50 mol% V: Si show that vanadia crystals are mostly aligned along the fiber axis. XPS shows an increase in vanadium contents at the surface, and XRD patterns exhibit an increase in the degree of crystallinity. A coaxial electrospinning scheme has successfully been employed to selectively place V2O5 in the skin layer.

  9. Sol-Gel Synthesis of Ordered β-Cyclodextrin-Containing Silicas.

    Science.gov (United States)

    Trofymchuk, Iryna Mykolaivna; Roik, Nadiia; Belyakova, Lyudmila

    2016-12-01

    New approaches for β-cyclodextrin-containing silicas synthesis were demonstrated. Materials with hexagonally ordered mesoporous structure were prepared by postsynthesis grafting and by co-condensation methods. β-Cyclodextrin activated by a N,N'-carbonyldiimidazole was employed for postsynthesis treatment of 3-aminopropyl-modified MCM-41 support as well as for sol-gel synthesis with β-cyclodextrin-containing organosilane and tetraethyl orthosilicate participation in the presence of cetyltrimethylammonium bromide. The successful incorporation of cyclic oligosaccharide moieties in silica surface layer was verified by means of FT-IR spectroscopy and chemical analysis. Obtained β-cyclodextrin-containing materials were characterized by X-ray diffraction, transmission electron microscopy, and low-temperature adsorption-desorption of nitrogen. In spite of commensurable loading of β-cyclodextrin groups attained by both proposed approaches (up to 0.028 μmol · m(-2)), it was found that co-condensation procedure provides uniform distribution of β-cyclodextrin functionalities in silica framework, whereas postsynthesis grafting results in modification of external surface of silica surface. Adsorption of benzene from aqueous solutions onto the surface of β-cyclodextrin-containing materials prepared by co-condensation method was studied as the function of time and equilibrium concentration. Langmuir and Freundlich models were used to evaluate adsorption processes and parameters. Adsorption experiments showed that β-cyclodextrin-containing silicas could be promising for the trace amount removal of aromatics from water.

  10. Sol-Gel Synthesis of Ordered β-Cyclodextrin-Containing Silicas

    Science.gov (United States)

    Trofymchuk, Iryna Mykolaivna; Roik, Nadiia; Belyakova, Lyudmila

    2016-03-01

    New approaches for β-cyclodextrin-containing silicas synthesis were demonstrated. Materials with hexagonally ordered mesoporous structure were prepared by postsynthesis grafting and by co-condensation methods. β-Cyclodextrin activated by a N, N'-carbonyldiimidazole was employed for postsynthesis treatment of 3-aminopropyl-modified MCM-41 support as well as for sol-gel synthesis with β-cyclodextrin-containing organosilane and tetraethyl orthosilicate participation in the presence of cetyltrimethylammonium bromide. The successful incorporation of cyclic oligosaccharide moieties in silica surface layer was verified by means of FT-IR spectroscopy and chemical analysis. Obtained β-cyclodextrin-containing materials were characterized by X-ray diffraction, transmission electron microscopy, and low-temperature adsorption-desorption of nitrogen. In spite of commensurable loading of β-cyclodextrin groups attained by both proposed approaches (up to 0.028 μmol · m-2), it was found that co-condensation procedure provides uniform distribution of β-cyclodextrin functionalities in silica framework, whereas postsynthesis grafting results in modification of external surface of silica surface. Adsorption of benzene from aqueous solutions onto the surface of β-cyclodextrin-containing materials prepared by co-condensation method was studied as the function of time and equilibrium concentration. Langmuir and Freundlich models were used to evaluate adsorption processes and parameters. Adsorption experiments showed that β-cyclodextrin-containing silicas could be promising for the trace amount removal of aromatics from water.

  11. Thickness controlled sol-gel silica films for plasmonic bio-sensing devices

    Science.gov (United States)

    Figus, Cristiana; Quochi, Francesco; Artizzu, Flavia; Saba, Michele; Marongiu, Daniela; Floris, Francesco; Marabelli, Franco; Patrini, Maddalena; Fornasari, Lucia; Pellacani, Paola; Valsesia, Andrea; Mura, Andrea; Bongiovanni, Giovanni

    2014-10-01

    Plasmonics has recently received considerable interest due to its potentiality in many fields as well as in nanobio-technology applications. In this regard, various strategies are required for modifying the surfaces of plasmonic nanostructures and to control their optical properties in view of interesting application such as bio-sensing, We report a simple method for depositing silica layers of controlled thickness on planar plasmonic structures. Tetraethoxysilane (TEOS) was used as silica precursor. The control of the silica layer thickness was obtained by optimizing the sol-gel method and dip-coating technique, in particular by properly tuning different parameters such as pH, solvent concentration, and withdrawal speed. The resulting films were characterized via atomic force microscopy (AFM), Fourier-transform (FT) spectroscopy, and spectroscopic ellipsometry (SE). Furthermore, by performing the analysis of surface plasmon resonances before and after the coating of the nanostructures, it was observed that the position of the resonance structures could be properly shifted by finely controlling the silica layer thickness. The effect of silica coating was assessed also in view of sensing applications, due to important advantages, such as surface protection of the plasmonic structure.

  12. Thickness controlled sol-gel silica films for plasmonic bio-sensing devices

    Energy Technology Data Exchange (ETDEWEB)

    Figus, Cristiana, E-mail: cristiana.figus@dsf.unica.it; Quochi, Francesco, E-mail: cristiana.figus@dsf.unica.it; Artizzu, Flavia, E-mail: cristiana.figus@dsf.unica.it; Saba, Michele, E-mail: cristiana.figus@dsf.unica.it; Marongiu, Daniela, E-mail: cristiana.figus@dsf.unica.it; Mura, Andrea; Bongiovanni, Giovanni [Dipartimento di Fisica - University of Cagliari, S.P. Km 0.7, I-09042 Monserrato (Canada) (Italy); Floris, Francesco; Marabelli, Franco; Patrini, Maddalena; Fornasari, Lucia [Dipartimento di Fisica - University of Pavia, Via Agostino Bassi 6, I-27100 Pavia (PV) (Italy); Pellacani, Paola; Valsesia, Andrea [Plasmore S.r.l. -Via Grazia Deledda 4, I-21020 Ranco (Vatican City State, Holy See) (Italy)

    2014-10-21

    Plasmonics has recently received considerable interest due to its potentiality in many fields as well as in nanobio-technology applications. In this regard, various strategies are required for modifying the surfaces of plasmonic nanostructures and to control their optical properties in view of interesting application such as bio-sensing, We report a simple method for depositing silica layers of controlled thickness on planar plasmonic structures. Tetraethoxysilane (TEOS) was used as silica precursor. The control of the silica layer thickness was obtained by optimizing the sol-gel method and dip-coating technique, in particular by properly tuning different parameters such as pH, solvent concentration, and withdrawal speed. The resulting films were characterized via atomic force microscopy (AFM), Fourier-transform (FT) spectroscopy, and spectroscopic ellipsometry (SE). Furthermore, by performing the analysis of surface plasmon resonances before and after the coating of the nanostructures, it was observed that the position of the resonance structures could be properly shifted by finely controlling the silica layer thickness. The effect of silica coating was assessed also in view of sensing applications, due to important advantages, such as surface protection of the plasmonic structure.

  13. Adsorption Characteristics of Water and Silica Gel System for Desalination Cycle

    KAUST Repository

    Cevallos, Oscar R.

    2012-07-01

    An adsorbent suitable for adsorption desalination cycles is essentially characterized by a hydrophilic and porous structure with high surface area where water molecules are adsorbed via hydrogen bonding mechanism. Silica gel type A++ possesses the highest surface area and exhibits the highest equilibrium uptake from all the silica gels available in the market, therefore being suitable for water desalination cycles; where adsorbent’s adsorption characteristics and water vapor uptake capacity are key parameters in the compactness of the system; translated as feasibility of water desalination through adsorption technologies. The adsorption characteristics of water vapor onto silica gel type A++ over a temperature range of 30 oC to 60 oC are investigated in this research. This is done using water vapor adsorption analyzer utilizing a constant volume and variable pressure method, namely the Hydrosorb-1000 instrument by Quantachrome. The experimental uptake data is studied using numerous isotherm models, i. e. the Langmuir, Tóth, generalized Dubinin-Astakhov (D-A), Dubinin-Astakhov based on pore size distribution (PSD) and Dubinin-Serpinski (D-Se) isotherm for the whole pressure range, and for a pressure range below 10 kPa, proper for desalination cycles; isotherms type V of the International Union of Pure and Applied Chemistry (IUPAC) classification were exhibited. It is observed that the D-A based on PSD and the D-Se isotherm models describe the best fitting of the experimental uptake data for desalination cycles within a regression error of 2% and 6% respectively. All isotherm models, except the D-A based on PSD, have failed to describe the obtained experimental uptake data; an empirical isotherm model is proposed by observing the behavior of Tóth and D-A isotherm models. The new empirical model describes the water adsorption onto silica gel type A++ within a regression error of 3%. This will aid to describe the advantages of silica gel type A++ for the design of

  14. Water repellent porous silica films by sol-gel dip coating method.

    Science.gov (United States)

    Rao, A Venkateswara; Gurav, Annaso B; Latthe, Sanjay S; Vhatkar, Rajiv S; Imai, Hiroaki; Kappenstein, Charles; Wagh, P B; Gupta, Satish C

    2010-12-01

    The wetting of solid surfaces by water droplets is ubiquitous in our daily lives as well as in industrial processes. In the present research work, water repellent porous silica films are prepared on glass substrate at room temperature by sol-gel process. The coating sol was prepared by keeping the molar ratio of methyltriethoxysilane (MTES), methanol (MeOH), water (H(2)O) constant at 1:12.90:4.74, respectively, with 2M NH(4)OH throughout the experiments and the molar ratio (M) of MTES/Ph-TMS was varied from 0 to 0.22. A simple dip coating technique is adopted to coat silica films on the glass substrates. The static water contact angle as high as 164° and water sliding angle as low as 4° was obtained for silica film prepared from M=0.22. The surface morphological studies of the prepared silica film showed the porous structure with pore sizes typically ranging from 200nm to 1.3μm. The superhydrophobic silica films prepared from M=0.22 retained their superhydrophobicity up to a temperature of 285°C and above this temperature the films became superhydrophilic. The porous and water repellent silica films are prepared by proper alteration of the Ph-TMS in the coating solution. The prepared silica films were characterized by surface profilometer, scanning electron microscopy (SEM), transmission electron microscopy (TEM), Fourier Transform Infrared (FT-IR) spectroscopy, humidity tests, chemical aging tests, static and dynamic water contact angle measurements.

  15. Increase of the final setting time of brushite cements by using chondroitin 4-sulfate and silica gel.

    Science.gov (United States)

    Tamimi-Mariño, F; Mastio, J; Rueda, C; Blanco, L; López-Cabarcos, E

    2007-06-01

    Chondroitin 4-sulfate (C4S) is a bioactive glycosaminoglycan with inductive properties in bone and tissue regeneration. Dicalcium phosphate dehydrate cements (known as brushite) are biocompatible and resorbable materials used in bone and dental surgery. In this study we analyzed the effect of C4S on the setting of a calcium phosphate cement and the properties of the resulting material. Brushite based cement powder was synthesised by mixing monocalcium phosphate with beta-tricalcium phosphate and sodium pyrophosphate. When the concentration of C4S, in the liquid added to the cement powder, was between 1 and 8% the cement final setting time increases. Furthermore, the cement diametral tensile strength remains unaffected when solutions with concentrations of C4S below 5% were used, but decreases at higher C4S concentrations. Calorimetric analysis showed that the cements prepared with C4S alone and in combination with silica gel have a greater content of hydrated water. We concluded from our study that the addition of small amounts of C4S increases the cement setting time without affecting its diametral tensile strength and at the same time improves the cement's hydrophilicity.

  16. Characterization of silica particles prepared via urease-catalyzed urea hydrolysis and activity of urease in sol-gel silica matrix

    Energy Technology Data Exchange (ETDEWEB)

    Kato, Katsuya, E-mail: katsuya-kato@aist.go.jp [National Institute of Advanced Industrial Science and Technology (AIST), 2266-98 Anagahora, Shimoshidami, Moriyama-ku, Nagoya 463-8560 (Japan); Nishida, Masakazu [National Institute of Advanced Industrial Science and Technology (AIST), 2266-98 Anagahora, Shimoshidami, Moriyama-ku, Nagoya 463-8560 (Japan); Ito, Kimiyasu; Tomita, Masahiro [Division of Chemistry for Materials, Graduate School of Engineering, Mie University, 1577 Kurimamachiya-cho, Tsu, Mie 514-8570 (Japan)

    2012-12-01

    Highlights: Black-Right-Pointing-Pointer Silica precipitation occurred via urease-catalytic reactions. Black-Right-Pointing-Pointer Higher urease activity for silica synthesis enables mesostructure of silica-urease composites. Black-Right-Pointing-Pointer Urease encapsulating in silica matrix retained high activity. - Abstract: Urease templated precipitation of silica synthesized by sol-gel chemistry produces a composite material allowing high urease activity. This study investigates the structural properties of the composite material that allow for the retention of the urease hydrolysis activity. Scanning (SEM) and transmission (TEM) electron microscopy reveal that the composite has a mesoporous structure composed of closely packed spherical structures {approx}20-50 nm in diameter. Brunauer-Emmett-Teller (BET) analysis revealed that the surface area and pore volume of the composite prepared under the conditions of 50 mM urea and 25 Degree-Sign C is relatively high (324 m{sup 2}/g and 1.0 cm{sup 3}/g). These values are equivalent to those of usual mesoporous silica materials synthesized from the self-assembly of triblock copolymers as organic templates. In addition, after encapsulating in a sol-gel silica matrix, urease retained high activity ({approx}90% of the activity compared with native urease). Our results suggest a new method for synthesizing mesoporous silica materials with highly tunable pore sizes and shapes under mild conditions.

  17. Inkjet printing of sol-gel synthesized hydrated tungsten oxide nanoparticles for flexible electrochromic devices.

    Science.gov (United States)

    Costa, Cláudia; Pinheiro, Carlos; Henriques, Inês; Laia, César A T

    2012-03-01

    Tungsten oxide nanoparticles were synthesized via a sol-gel route using metallic tungsten as precursor, and were printed on a flexible electrode using inkjet printing in order to build solid-state electrochromic cells. Several spectroscopic techniques were used to characterize and compare tungsten oxide particles obtained from different origins. FTIR, Raman and X-ray diffraction spectroscopic measurements showed that the sol-gel synthesis described here produces nanoparticles mainly in an amorphous state with hexagonal crystalline domains and allowed the analysis of the hydration extent of those nanoparticles. The size was measured combining dynamic light scattering, sedimentation, and microscopic techniques (AFM), showing a consistent size of about 200 nm. The tungsten oxide nanoparticles were used to produce an ink formulation for application in inkjet printing. Solid-state electrochromic devices were assembled at room temperature, without sintering the tungsten oxide printed films, showing excellent contrast between on/off states. Electrochemical characterization of those films is described using cyclic voltammetry. The devices were then tested through spectroelectrochemistry by Visible/NIR absorption spectroscopy (400-2200 nm range), showing a dual spectroscopic response depending on the applied voltage. This phenomenon is attributed to the presence of two different crystalline states in accordance with results obtained from the spectroscopic characterization of the nanoparticles. The electrochromic cells had a good cycling stability showing high reversibility and a cyclability up to more than 50,000 cycles with a degradation of 25%. © 2012 American Chemical Society

  18. Synthesis of Silica Nanoparticles by Sol-Gel: Size-Dependent Properties, Surface Modification, and Applications in Silica-Polymer Nanocomposites—A Review

    Directory of Open Access Journals (Sweden)

    Ismail Ab Rahman

    2012-01-01

    Full Text Available Application of silica nanoparticles as fillers in the preparation of nanocomposite of polymers has drawn much attention, due to the increased demand for new materials with improved thermal, mechanical, physical, and chemical properties. Recent developments in the synthesis of monodispersed, narrow-size distribution of nanoparticles by sol-gel method provide significant boost to development of silica-polymer nanocomposites. This paper is written by emphasizing on the synthesis of silica nanoparticles, characterization on size-dependent properties, and surface modification for the preparation of homogeneous nanocomposites, generally by sol-gel technique. The effect of nanosilica on the properties of various types of silica-polymer composites is also summarized.

  19. Strong Static Magnetic Fields Increase the Gel Signal in Partially Hydrated DPPC/DMPC Membranes

    Directory of Open Access Journals (Sweden)

    Jennifer Tang

    2015-09-01

    Full Text Available NIt was recently reported that static magnetic fields increase lipid order in the hydrophobic membrane core of dehydrated native plant plasma membranes [Poinapen, Soft Matter 9:6804-6813, 2013]. As plasma membranes are multicomponent, highly complex structures, in order to elucidate the origin of this effect, we prepared model membranes consisting of a lipid species with low and high melting temperature. By controlling the temperature, bilayers coexisting of small gel and fluid domains were prepared as a basic model for the plasma membrane core. We studied molecular order in mixed lipid membranes made of dimyristoyl-sn-glycero-3-phosphocholine (DMPC and dipalmitoyl-sn-glycero-3-phosphocholine (DPPC using neutron diffraction in the presence of strong static magnetic fields up to 3.5 T. The contribution of the hydrophobic membrane core was highlighted through deuterium labeling the lipid acyl chains. There was no observable effect on lipid organization in fluid or gel domains at high hydration of the membranes. However, lipid order was found to be enhanced at a reduced relative humidity of 43%: a magnetic field of 3.5 T led to an increase of the gel signal in the diffraction patterns of 5%. While all biological materials have weak diamagnetic properties, the corresponding energy is too small to compete against thermal disorder or viscous effects in the case of lipid molecules. We tentatively propose that the interaction between the fatty acid chains’ electric moment and the external magnetic field is driving the lipid tails in the hydrophobic membrane core into a better ordered state.

  20. Synthesis and characterization of nanocomposite powders of calcium phosphate/silica-gel; Sintese e caracterizacao de pos nanoestruturados de fosfato de calcio/silica-gel

    Energy Technology Data Exchange (ETDEWEB)

    Muller, D.T.; Delima, S.A. [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Dept. de Engenharia Mecanica; Santos, R.B.M.; Camargo, N.H.A., E-mail: dem2nhac@joinville.udesc.b [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Programa de Pos Graduacao em Ciencia e Engenharia de Materiais

    2009-07-01

    In the recent years ceramics of calcium phosphate are pointed out as an outstanding material in substitution and regeneration in defects from osseous tissue, in reason of their similar mineralogical characteristics of apatite of bone structure. However, the challenge with phosphate calcium ceramics find out about the mechanical properties and the development of biomaterials similar of the bone structure, what sometimes is not so easy, about fragile materials. The aim of this work focused in synthesis and characterization nanocomposites powders of calcium phosphate/silica-gel with percentages 1, 2, 3 e 5% of nanometric silica. The method synthesis used for the compositions elaboration was dissolution-precipitation. The presented results are related with the optimization to method elaboration of nanostructured powders, the mineralogical characterization with X-ray diffraction, thermal behavior with thermal differential analysis, differential scanning calorimetry here is ADT and dilatometer. The scanning electronic microscopy was used to help of morphological characterization the nanostructured powders and the surfaces from body test recovered from the mechanical test. (author)

  1. Advanced treatment of swine wastewater using an agent synthesized from amorphous silica and hydrated lime.

    Science.gov (United States)

    Tanaka, Yasuo; Hasegawa, Teruaki; Sugimoto, Kiyomi; Miura, Keiichi; Aketo, Tsuyoshi; Minowa, Nobutaka; Toda, Masaya; Kinoshita, Katsumi; Yamashita, Takahiro; Ogino, Akifumi

    2014-01-01

    Advanced treatment using an agent synthesized from amorphous silica and hydrated lime (M-CSH-lime) was developed and applied to swine wastewater treatment. Biologically treated wastewater and M-CSH-lime (approximately 6 w/v% slurry) were fed continuously into a column-shaped reactor from its bottom. Accumulated M-CSH-lime gradually formed a bed layer. The influent permeated this layer and contacted the M-CSH-lime, and the treatment reaction progressed. Treated liquid overflowing from the top of the reactor was neutralized with CO₂gas bubbling. The colour removal rate approximately exceeded 50% with M-CSH-lime addition rates of > 0.15 w/v%. The removal rate of PO(3⁻)(4) exceeded 80% with the addition of>0.03 w/v% of M-CSH-lime. The removal rates of coliform bacteria and Escherichia coli exceeded 99.9% with > 0.1 w/v%. Accumulated M-CSH-lime in the reactor was periodically withdrawn from the upper part of the bed layer. The content of citric-acid-soluble P₂O₅ in the recovered matter was>15% when the weight ratio of influent PO(3⁻)(4) -P to added M-CSH-lime was > 0.15. This content was comparable with commercial phosphorus fertilizer. The inhibitory effect of recovered M-CSH-lime on germination and growth of leafy vegetable komatsuna (Brassica rapa var. perviridis) was evaluated by an experiment using the Neubauer's pot. The recovered M-CSH-lime had no negative effect on germination and growth. These results suggest that advanced water treatment with M-CSH-lime was effective for simultaneous removal of colour, [Formula: see text] and coliform bacteria at an addition rate of 0.03-0.15 w/v%, and that the recovered M-CSH-lime would be suitable as phosphorus fertilizer.

  2. Capture of Co(II) from its aqueous EDTA-chelate by DTPA-modified silica gel and chitosan.

    Science.gov (United States)

    Repo, Eveliina; Malinen, Leena; Koivula, Risto; Harjula, Risto; Sillanpää, Mika

    2011-03-15

    The adsorption of Co(II) by diethylenetriaminepentaacetic acid (DTPA)-modified silica gel and chitosan in the presence of EDTA and other interfering species was studied. Co(II) removal ranged from 93% to 96% from the solutions where Co(II) was totally chelated by EDTA. The amount of oxalate or Fe(II) did not affect the adsorption of Co(II) in the case of DTPA-chitosan. However, increasing the amount of oxalate enhanced the adsorption performance of DTPA-silica gel, probably due to the formation of new active sites on the silica gel surface. DTPA-chitosan was also effective in simulated decontamination solutions. For DTPA-silica gel, the rate of adsorption of free Co(II) was controlled by pore diffusion, but the rate of adsorption of Co(II)EDTA was controlled by the surface chelation reaction, which was attributed to the inhibited diffusion of Co(II)EDTA inside the silica gel mesopores. However, the macroporous structure of DTPA-chitosan enabled pore diffusion of both Co(II) and Co(II)EDTA. The equilibrium isotherms of DTPA-silica gel were best described by a BiLangmuir model, in which there are two different adsorption sites on the silica gel surface assigned to different speciations of DTPA. For DTPA-chitosan, the data fit best with a Sips model, which indicates system heterogeneity. Finally, measurements with capillary electrophoresis showed an increase in dissolved EDTA during adsorption, demonstrating the ability of DTPA-modified adsorbents to release Co(II) from its EDTA chelate. This promising result can provide a basis for applying the studied materials to the treatment of water effluents containing Co(II) chelated by EDTA by a simple one-step adsorption process. Copyright © 2011 Elsevier B.V. All rights reserved.

  3. The relationship between the morphology of brushite crystals grown rapidly in silica gel and its structure

    Science.gov (United States)

    Ohta, M.; Tsutsumi, M.

    1982-02-01

    The morphology of brushite, CaHPO 4 · 2 H 2O, provides some basic information on biological mineralization. The growth, morphology and surface structures of brushite crystals grown at fairly high growth rates in silica gel at 37°C in the initial pH range of 4 to 6 (the final pH range of about 3.2 to 4.7) have been investigated. Their preferred growth direction is [101]: there is a marked tendency for calcium and phosphate ions in the gel to attach to (111) or (101) surfaces; inclusions derived from silica gel are also incorporated, mainly along the [101] direction in the initial stage of crystal growth and at higher pH values. The following order of "edge strength", which refers to a sort of resistance of crystal edge against getting out of its shape, was obtained experimentally for the edges parallel to the (010) face of brushite: [101] ⪆ [201] > [001] ⪆ [100]. The relationship between the above order and the structure of corrugated sheets with composition [CaHPO 4] is also discussed.

  4. Effect of Catalyst on the Formation of Silica Coating on Nickel Substrate by Sol -Gel Processing

    Institute of Scientific and Technical Information of China (English)

    Ali Ghasemi; F.Ashrafizadeh; M.A.Golozar; Ali Ashrafi

    2004-01-01

    In this research work silica coating was produced on nickel substrates by a sol-gel process. In order to increase the rate of hydrolysis and to reduce the rate of polymerization several acid catalysts including nitric acid-hydrochloric acid,acetic acid, hydrochloric acid and nitric acid were add to silica sol. Conversely, in order to control the rate of hydrolysis and to increase the rate of polymerization, basic catalyst of ammonia and ammonia hydroxyl were introduced in to the solution.Nickel specimens of known surface roughness were chemically cleaned and prepared by dipping in the sols. In order to produce a suitable silica coating the drying and firing cycles were optimized on these substrates. The structure and uniformity of the coatings produced were examined by scanning electron microscopy. Coatings composition was determined using glow discharge optical spectroscopy and EDAX microanalysis. Experimental result showed that hydrochloric acid, acetic acid, ammonia and acetic acid - ammonia are suitable catalytic agents for silica coating formation on nickel type substrate.

  5. Shock-wave compression of silica gel as a model material for comets

    Science.gov (United States)

    Arasuna, Akane; Okuno, Masayuki; Chen, Liliang; Mashimo, Tsutomu; Okudera, Hiroki; Mizukami, Tomoyuki; Arai, Shoji

    2016-07-01

    A shock-wave compression experiment using synthesized silica gel was investigated as a model for a comet impact event on the Earth's surface. The sample shocked at 20.7 GPa showed considerable structural changes, a release of water molecules, and the dehydration of silanol (Si-OH) that led to the formation of a new Si-O-Si network structure containing larger rings (e.g., six-membered ring of SiO4 tetrahedra). The high aftershock temperature at 20.7 GPa, which could be close to 800 °C, influenced the sample structure. However, some silanols, which were presumed to be the mutually hydrogen-bonded silanol group, remained at pressures >20.7 GPa. This type of silanol along with a small number of water molecules may remain even after shock compression at 30.9 GPa, although the intermediate structure of the sample recovered was similar to that of silica glass.

  6. Fluorescence metrology of silica sol-gels - The effect of D2O and inorganic salts

    Indian Academy of Sciences (India)

    D J S Birch; C D Geddes

    2000-06-01

    We have developed a new method for measuring in-situ the growth of the nanometre-size silica particles which lead to the formation of sol-gel glasses. This technique is based on the decay of fluorescence polarisation anisotropy due to Brownian rotation of dye molecules bound to the particles. Results to date give near ångstrom resolution and demonstrate the feasibility of the approach both for providing industrial quality control and helping fundamental research. Our approach has several key advantages over traditional techniques for nanometre metrology, such as small angle X-ray and neutron scattering and electron microscopy. In this paper we present silica particle growth dynamics in a hydrogel as detected by two near-infrared dyes, the effect of adding D2O on the hydrodynamic radius and the effect of salt addition.

  7. Ultraviolet laser-induced damage on fused silica substrate and its sol-gel coating.

    Science.gov (United States)

    Li, Xiaoguang; Gross, Mark; Green, Katie; Oreb, Bob; Shen, Jun

    2012-06-15

    A comparative study of the laser-induced damage thresholds (LIDTs) of fused silica substrates and their sol-gel silica coatings was carried out with 355 nm laser irradiation. Chemical etching and superpolishing were employed in different ways to improve the substrate. The laser damage tests showed that the coated substrate was no more susceptible to laser damage than the bare substrate, showing that the substrate quality was the dominant factor limiting the LIDT for UV irradiation. In addition, it was found that high value of substrate microroughness was more harmful to the LIDT of the coated than the bare substrate, and that a proper combination of etching and superpolishing can optimize the LIDT.

  8. Europium incorporated in silica matrix obtained by sol-gel: luminescent materials

    Directory of Open Access Journals (Sweden)

    Eduardo José Nassar

    2003-12-01

    Full Text Available In this work we report some aspects of the chemistry involved in the preparation of modified silicon oxide by the sol-gel process. Europium III compounds were used as luminescent probe. An organic-inorganic hybrid was obtained by hydrolysis of tetraethylorthosilicate (TEOS and 3-aminopropyltriethoxysilane (APTS. The Eu III compounds were added in different ways. In the first, silica was prepared in the presence of Eu III, and in the second, Eu III was added on the silica surface. These materials were studied by luminescence, infrared spectroscopy and termogravimetric analysis. The results obtained for the hybrid material show different behavior for Eu III emission, which could be excited by the antenna effect and the influence of the surrounding in the luminescence quenching. The thermogravimetric data present different mass loss in samples to range temperature 50 - 150 °C. Thermogravimetric and infrared spectra showed that inorganic polymers incorporated the organic part.

  9. The effects of silica fume and hydrated lime on the strength development and durability characteristics of concrete under hot water curing condition

    Directory of Open Access Journals (Sweden)

    Hamza Ali

    2017-01-01

    Full Text Available Sustainability is considered to be highly important for preserving continued industrial growth and human development. Concrete, being the world’s largest manufacturing material comprises cement as an essential binding component for strength development. However, excessive production of cement due to high degree of construction practices around the world frames cement as a leading pollutant of releasing significant amounts of CO2 in the atmosphere. To overcome this environmental degradation, silica fume and hydrated lime are used as partial replacements to cement. This paper begins with the examination of the partial replacement levels of hydrated lime and silica fume in concrete and their influence on the mechanical properties and durability characteristics of concrete. The effect of hot water curing on concrete incorporated with both silica fume and hydrated lime is also investigated in this paper. The results reported in this paper show that the use of silica fume as a partial replacement material improved both the mechanical properties and durability characteristics of concrete due to the formation of calcium silica hydrate crystals through the pozzolanic reaction. Although the hydrated lime did not significantly contribute in the development of strength, its presence enhanced the durability of concrete especially at long-term. The results also showed that hot water curing enhanced the strength development of concrete incorporated with silica fume due to the accelerated rate of both the hydration and pozzolanic reaction that takes place between silica fume and calcium hydroxide of the cement matrix particularly at early times. The results reported in this paper have significant contribution in the development of sustainable concrete. The paper does not only address the use of alternative binders as a partial replacement material in concrete but also suggest proper curing conditions for the proposed replacement materials. These practices

  10. Aplicação e modificação química da sílica gel obtida de areia Aplication and chemical modification of silica-gel obtained from sand

    Directory of Open Access Journals (Sweden)

    Alexandre G. S. Prado

    2005-06-01

    Full Text Available The silica gel was obtained from sand and its surface was modified with POCl3 to produce Si-Cl bonds on the silica surface. Ethylenediamine was covalently bonded onto the chlorinated silica surface. The adsorption of the chlorides of divalent cobalt, nickel and copper was qualitatively studied to show that the bonding of ethylenediamine onto the silica gel surface produces a solid base capable of chelating metal ions from solution. The experiments illustrate the extraction of silica gel, its reactivity, the development of modified surfaces and its application in removing metal ions from water and are deigned for undergraduate inorganic chemistry laboratories.

  11. The Applicability of Acoustic Wave Propagation Models to Silica Sols and Gels.

    Science.gov (United States)

    Holmes; Challis

    1999-08-01

    Acoustic attenuation and phase velocity in the frequency range 2-50 MHz have been measured in a series of silica sols and gels with particle sizes in the range 12-30 nm, and concentrations in the range 5-40% (w/w). Results have been compared with both scattering and hydrodynamic models of acoustic propagation in colloids. Differences between measured and simulated results indicate that present models are inadequate for very small particle sizes and small particle separations (<50 nm), where very high number concentrations of scatterers are present. Copyright 1999 Academic Press.

  12. Computational Fluid Dynamics Modelling and Experimental Study on a Single Silica Gel Type B

    Directory of Open Access Journals (Sweden)

    John White

    2012-01-01

    Full Text Available The application of computational fluid dynamics (CFDs in the area of porous media and adsorption cooling system is becoming more practical due to the significant improvement in computer power. The results from previous studies have shown that CFD can be useful tool for predicting the water vapour flow pattern, temperature, heat transfer and flow velocity and adsorption rate. This paper investigates the effect of silica gel granular size on the water adsorption rate using computational fluid dynamics and gravimetric experimental (TGA method.

  13. Synthesis of all-silica zeolites from highly concentrated gels containing hexamethonium cations

    KAUST Repository

    Liu, Xiaolong

    2012-07-01

    A pure and highly crystalline all-silica EU-1 zeolite has been obtained from the crystallization of gels containing very low water contents in the presence of hexamethonium cations. Decreasing the water content in the gel down to H 2O/Si < 1 inhibited the formation of ZSM-48, which is usually observed under more diluted standard crystallization conditions. Moreover, addition of NH 4F to the synthesis led to the formation of "half-fluorinated" ITQ-13 in which fluoride anions occupied only the center of D4R cages. In larger cages, the charge of the template was compensated by framework connectivity defects, clearly demonstrating once more the essential role of F - in the formation of D4R units. The formation of such hybrid (F,OH) is particularly interesting from a synthesis point of view, particularly for understanding the respective roles of fluoride and hydroxide anions in the crystallization process. © 2012 Elsevier Inc. All rights reserved.

  14. Preparation, characterization and photocatalytic activity of manganese doped TiO(2) immobilized on silica gel.

    Science.gov (United States)

    Xu, Yuehua; Lei, Bo; Guo, Laiqiu; Zhou, Wuyi; Liu, Youqin

    2008-12-15

    A series of Mn-TiO(2)/SiO(2) (silica gel loaded with manganese doped TiO(2)) photocatalysts have been prepared by sol-gel method, and characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and X-ray photoelectron spectroscopy (XPS). Photocatalytic activities were enhanced in photocatalytic degradation of methyl orange over Mn-TiO(2)/SiO(2). XPS analysis shows that a Ti-O-Si or Ti-O-Mn bond is formed on the surface of photocatalyst. Mn is doped as a mixture of Mn(2+) and Mn(3+) on the surface of 1.0mol% Mn-TiO(2)/SiO(2). Mn(3+) appears to trap electrons and prohibit the electron-hole recombination. The electrons trapped in Mn(3+) site are subsequently transferred to the adsorbed O(2). As a result, the combination of the electron-hole pair was reduced.

  15. Durable superhydrophobic and antireflective surfaces by trimethylsilanized silica nanoparticles-based sol-gel processing.

    Science.gov (United States)

    Manca, Michele; Cannavale, Alessandro; De Marco, Luisa; Aricò, Antonino S; Cingolani, Roberto; Gigli, Giuseppe

    2009-06-02

    We present a robust and cost-effective coating method to fabricate long-term durable superhydrophobic andsimultaneouslyantireflective surfaces by a double-layer coating comprising trimethylsiloxane (TMS) surface-functionalized silica nanoparticles partially embedded into an organosilica binder matrix produced through a sol-gel process. A dense and homogeneous organosilica gel layer was first coated onto a glass substrate, and then, a trimethylsilanized nanospheres-based superhydrophobic layer was deposited onto it. After thermal curing, the two layers turned into a monolithic film, and the hydrophobic nanoparticles were permanently fixed to the glass substrate. Such treated surfaces showed a tremendous water repellency (contact angle = 168 degrees ) and stable self-cleaning effect during 2000 h of outdoor exposure. Besides this, nanotextured topology generated by the self-assembled nanoparticles-based top layer produced a fair antireflection effect consisting of more than a 3% increase in optical transmittance.

  16. Effectiveness of silica based sol-gel microencapsulation method for odorants and flavors leading to sustainable environment.

    Science.gov (United States)

    Ashraf, Muhammad Aqeel; Khan, Aysha Masood; Ahmad, Mushtaq; Sarfraz, Maliha

    2015-01-01

    Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol-gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol-gel SiO2 is non-toxic and safe, whereas the sol-gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped active agents, thereby broadening the practical utilization of chemically unstable essential oils (EOs). Reviewing progress in the fabrication of diverse odorant and flavored sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits.

  17. Effectiveness of silica based Sol-gel microencapsulation Method for odorants and flavours leading to sustainable Environment

    Directory of Open Access Journals (Sweden)

    Muhammad Aqeel eAshraf

    2015-08-01

    Full Text Available Microencapsulation has become a hot topic in chemical research. Technology mainly used for control release and protection purposes. The sol–gel micro encapsulation approach for fragrance and aroma in porous silica-based materials leads to sustainable odorant and flavored materials with novel and unique beneficial properties. Sol-gel encapsulation of silica based micro particles considered economically cheap as capital investment in manufacturing is very low and environmentally friendly. Amorphous sol–gel SiO2 is non-toxic and safe, whereas the sol–gel entrapment of delicate chemicals in its inner pores results in pronounced chemical and physical stabilization of the entrapped actives, thereby broadening the practical utilization of chemically unstable essential oils. Reviewing progress in the fabrication of diverse odorant and flavoured sol-gels, shows us how different synthetic strategies are appropriate for practical application with important health and environmental benefits.

  18. Generation of a mesoporous silica MSU shell onto solid core silica nanoparticles using a simple two-step sol-gel process.

    Science.gov (United States)

    Allouche, Joachim; Dupin, Jean-Charles; Gonbeau, Danielle

    2011-07-14

    Silica core-shell nanoparticles with a MSU shell have been synthesized using several non-ionic poly(ethylene oxide) based surfactants via a two step sol-gel method. The materials exhibit a typical worm-hole pore structure and tunable pore diameters between 2.4 nm and 5.8 nm.

  19. Preparation and Characterization of Titania-silica Composite Particles by Pechini Sol-gel Method

    Directory of Open Access Journals (Sweden)

    Wu Yuanting

    2016-01-01

    Full Text Available Two Pechini sol-gel processes were used to prepare titania-silica composite particles. The dynamic oxidation behavior of the TiO2-SiO2 powders has been characterized by thermogravimetry-differential scanning calorimetry (TG-DTG-DSC. The crystal phase and microstructure of the composite particles were investigated by X-ray diffraction (XRD and field emission scanning electron microscope (FE-SEM. The effects of Si:Ti molar ratio and sol-gel process on the TiO2-SiO2 powders were studied. The preparation of the polymeric precursors can influence the morphology of obtained TiO2-SiO2 composite particles. The spherical TiO2-SiO2 composite particles which are 20 nm~400 nm in diameter appear in gel-1 system. However, the TiO2-SiO2 powders obtained by gel-2 system are irregular in shape and 2~15 μm in diameter which show a loose porous structure consisted of very fine granules.

  20. Kinetic modeling of aldehyde adsorption rates on bare and aminopropylsilyl-modified silica gels by ultra-rapid-scanning fourier transform infrared spectrometry.

    Science.gov (United States)

    Yang, Husheng; Weinstock, Benjamin A; Hirsche, Blayne L; Griffiths, Peter R

    2005-04-26

    Enhancements of a model capable of precisely defining rates of adsorption in terms of a Langmuir isotherm and determined from infrared and pressure data collected in the millisecond time regime are described in detail. Rates of adsorption are determined for formaldehyde and acetaldehyde exposed to bare and aminopropylsilyl-derivatized silica gel. The model fits the collected data by varying the number of adsorption sites and the adsorption and desorption rate constants and determines the best fit based on the measured IR absorbance, partial pressure, exposure backpressure, number of adsorption sites, and time. The rate of adsorption onto irregular-shaped silica gel was faster than the rate onto the corresponding spherical silica gel. Formaldehyde was adsorbed more efficiently than acetaldehyde on APS silica gel than on bare silica gel, whereas acetaldehyde was adsorbed more efficiently than formaldehyde on underivatized silica, indicating the possibility that formaldehyde is adsorbed through the formation of a Schiff base.

  1. Microwave material characterization of alkali-silica reaction (ASR) gel in cementitious materials

    Science.gov (United States)

    Hashemi, Ashkan

    Since alkali-silica reaction (ASR) was recognized as a durability challenge in cement-based materials over 70 years ago, numerous methods have been utilized to prevent, detect, and mitigate this issue. However, quantifying the amount of produced ASR byproducts (i.e., ASR gel) in-service is still of great interest in the infrastructure industry. The overarching objective of this dissertation is to bring a new understanding to the fundamentals of ASR formation from a microwave dielectric property characterization point-of-view, and more importantly, to investigate the potential for devising a microwave nondestructive testing approach for ASR gel detection and evaluation. To this end, a comprehensive dielectric mixing model was developed with the potential for predicting the effective dielectric constant of mortar samples with and without the presence of ASR gel. To provide pertinent inputs to the model, critical factors on the influence of ASR gel formation on dielectric and reflection properties of several mortar samples were investigated at R, S, and X-band. Effects of humidity, alkali content, and long-term curing conditions on ASR-prone mortars were also investigated. Additionally, dielectric properties of chemically different synthetic ASR gel were also determined. All of these, collectively, served as critical inputs to the mixing model. The resulting developed dielectric mixing model has the potential to be further utilized to quantify the amount of produced ASR gel in cement-based materials. This methodology, once becomes more mature, will bring new insight to the ASR reaction, allowing for advancements in design, detection and mitigation of ASR, and eventually has the potential to become a method-of-choice for in-situ infrastructure health-monitoring of existing structures.

  2. Synthesis of sugar-based silica gels by copper-catalysed azide-alkyne cycloaddition via a single-step azido-activated silica intermediate and the use of the gels in hydrophilic interaction chromatography.

    Science.gov (United States)

    Moni, Lisa; Ciogli, Alessia; D'Acquarica, Ilaria; Dondoni, Alessandro; Gasparrini, Francesco; Marra, Alberto

    2010-05-17

    Novel sugar-based silica gels were prepared by exploiting the copper-catalysed azide-alkyne cycloaddition (CuAAC) of two different sugar alkynes, namely, ethynyl C-galactoside 1 and propargyl O-lactoside 2, with new single-step azido-activated silica gels. The fully characterised stationary phases were generally used for hydrophilic interaction chromatography (HILIC), with particular application in the stereoselective separation of monosaccharides. Dynamic HILIC (DHILIC) experiments were performed to evaluate the influence of mutarotation on the chromatographic peak shapes of two interconverting sugar anomers. The potential of such materials was shown in the separation of other highly polar compounds, including amino acids and flavonoids.

  3. Modeling the supercritical desorption of orange essential oil from a silica-gel bed

    Directory of Open Access Journals (Sweden)

    Silva E.A.

    2000-01-01

    Full Text Available One of the most important byproducts of the orange juice industry is the oil phase. This is a mixture of terpenes, alcohols, and aldehydes, dissolved in approximately 96% limonene. To satisfactorily use oil phase as an ingredient in the food and cosmetics industries separation of the limonene is required. One possibility is to use a fixed bed of silica gel to remove the light or aroma compounds from the limonene. The aroma substances are then extracted from the bed of silica gel using supercritical carbon dioxide. This work deals with the modeling of the desorption step of the process using mass balance equations coupled with the Langmuir equilibrium isotherm. Data taken from the literature for the overall extraction curves were used together with empirical correlations to calculate the concentration profile of solute in the supercritical phase at the bed outlet. The system of equations was solved by the finite volume technique. The overall extraction curves calculated were in good agreement with the experimental ones.

  4. Experimental comparison of adsorption characteristics of silica gel and zeolite in moist air

    Science.gov (United States)

    Xin, F.; Yuan, Z. X.; Wang, W. C.; Du, C. X.

    2016-05-01

    In this work, the macro adsorption characteristic of water vapor by the allochroic silica gel and the zeolite 5A and ZSM-5 were investigated experimentally. BET analysis method presented the difference of the porosity, the micro pore volume, and the specific surface area of the material. The dynamic and the equilibrium characteristics of the sample were measured thermo-gravimetrically in the moist air. In general, the ZSM-5 zeolite showed an inferior feature of the adsorption speed and the equilibrium concentration to the others. By comparison to the result of SAPO-34 zeolite in the open literature, the 5A zeolite showed some superiorities of the adsorption. The equilibrium concentration of the ZSM-5 zeolite was higher than that of the SAPO-34 calcined in the nitrogen, whereas it was lower than that calcined in the air. The adsorption isotherm was correlated and the relation of the isotherm to the microstructure of the material was discussed. With more mesopore volume involved, the zeolite presented an S-shaped isotherm in contrast to the exponential isotherm of the silica gel. In addition, the significance of the S-shaped isotherm for the application in adsorption heat pump has also been addressed.

  5. Experimental comparison of adsorption characteristics of silica gel and zeolite in moist air

    Science.gov (United States)

    Xin, F.; Yuan, Z. X.; Wang, W. C.; Du, C. X.

    2017-02-01

    In this work, the macro adsorption characteristic of water vapor by the allochroic silica gel and the zeolite 5A and ZSM-5 were investigated experimentally. BET analysis method presented the difference of the porosity, the micro pore volume, and the specific surface area of the material. The dynamic and the equilibrium characteristics of the sample were measured thermo-gravimetrically in the moist air. In general, the ZSM-5 zeolite showed an inferior feature of the adsorption speed and the equilibrium concentration to the others. By comparison to the result of SAPO-34 zeolite in the open literature, the 5A zeolite showed some superiorities of the adsorption. The equilibrium concentration of the ZSM-5 zeolite was higher than that of the SAPO-34 calcined in the nitrogen, whereas it was lower than that calcined in the air. The adsorption isotherm was correlated and the relation of the isotherm to the microstructure of the material was discussed. With more mesopore volume involved, the zeolite presented an S-shaped isotherm in contrast to the exponential isotherm of the silica gel. In addition, the significance of the S-shaped isotherm for the application in adsorption heat pump has also been addressed.

  6. Immobilization of Cyclooxygenase-2 on Silica Gel Microspheres: Optimization and Characterization

    Directory of Open Access Journals (Sweden)

    Qian Shi

    2015-11-01

    Full Text Available In this study, immobilized COX-2 was successfully constructed through glutaraldehyde-mediated covalent coupling on functional silica gel microspheres. The optimum conditions, properties, and morphological characteristics of the immobilized COX-2 were investigated. The optimal immobilization process was as follows: about 0.02 g of aminated silica gel microspheres was activated by 0.25% GA solution for 6 h and mixed with 5 U of free recombinant COX-2 solution. Then, the mixture was shaken for 8 h at 20 °C. Results showed that the immobilized COX-2 produced by this method exhibited excellent biocatalytic activity, equivalent to that of free COX-2 under the test conditions employed. The best biocatalytic activity of immobilized COX-2 appeared at pH 8.0 and still maintained at about 84% (RSD < 7.39%, n = 3 at pH 10.0. For temperature tolerance, immobilized COX-2 exhibited its maximum biocatalytic activity at 40 °C and about 68% (RSD < 6.99%, n = 3 of the activity was maintained at 60 °C. The immobilized COX-2 retained over 85% (RSD < 7.26%, n = 3 of its initial biocatalytic activity after five cycles, and after 10 days storage, the catalytic activity of immobilized COX-2 still maintained at about 95% (RSD < 3.08%, n = 3. These characteristics ensured the convenient use of the immobilized COX-2 and reduced its production cost.

  7. Mesoporous sol-gel silica cladding for hybrid TiO2/electro-optic polymer waveguide modulators.

    Science.gov (United States)

    Enami, Yasufumi; Kayaba, Yasuhisa; Luo, Jingdong; Jen, Alex K-Y

    2014-06-30

    We report the efficient poling of an electro-optic (EO) polymer in a hybrid TiO(2)/electro-optic polymer multilayer waveguide modulator on mesoporous sol-gel silica cladding. The mesoporous sol-gel silica has nanometer-sized pores and a low refractive index of 1.24, which improves mode confinement in the 400-nm-thick EO polymer film in the modulators and prevents optical absorption from the lower Au electrode, thereby resulting in a lower half-wave voltage of the modulators. The half-wave voltage (Vπ) of the hybrid modulator fabricated on the mesoporous sol-gel silica cladding is 6.0 V for an electrode length (Le) of 5 mm at a wavelength of 1550 nm (VπLe product of 3.0 V·cm) using a low-index guest-host EO polymer (in-device EO coefficient of 75 pm/V).

  8. Adsorption enhancement of elemental mercury onto sulphur-functionalized silica gel adsorbents.

    Science.gov (United States)

    Johari, Khairiraihanna; Saman, Norasikin; Mat, Hanapi

    2014-01-01

    In this study, elemental mercury (EM) adsorbents were synthesized using tetraethyl orthosilicate (TEOS) and 3-mercaptopropyl trimethoxysilane as silica precursors. The synthesized silica gel (SG)-TEOS was further functionalized through impregnation with elemental sulphur and carbon disulphide (CS2). The SG adsorbents were then characterized by using scanning electron microscope, Fourier transform infra-red spectrophotometer, nitrogen adsorption/desorption, and energy-dispersive X-ray diffractometer. The EM adsorption of the SG adsorbents was determined using fabricated fixed-bed adsorber. The EM adsorption results showed that the sulphur-functionalized SG adsorbents had a greater Hgo breakthrough adsorption capacity, confirming that the presence of sulphur in silica matrices can improve Hgo adsorption performance due to their high affinity towards mercury. The highest Hgo adsorption capacity was observed for SG-TEOS(CS2) (82.62 microg/g), which was approximately 2.9 times higher than SG-TEOS (28.47 microg/g). The rate of Hgo adsorption was observed higher for sulphur-impregnated adsorbents, and decreased with the increase in the bed temperatures.

  9. Sliding behavior of water drops on sol-gel derived hydrophobic silica films

    Energy Technology Data Exchange (ETDEWEB)

    Latthe, Sanjay S.; Dhere, Sunetra L. [Air Glass Laboratory, Department of Physics, Shivaji University, Kolhapur 416 004, Maharashtra (India); Kappenstein, Charles [University of Poitiers, Laboratory of Catalysis in Organic Chemistry, LA CCO, UMR CNRS 6503, Poitiers-86000 (France); Imai, Hiroaki [Faculty of Science and Technology, Keio University, 3-14-1, Hiyoshi, Kohoku-ku, Yokohama 223-8522 (Japan); Ganesan, V. [CSR, Indore Centre, University Campus, Khandwa Road, Indore- 452 017, Madhyapradesh (India); Rao, A. Venkateswara, E-mail: avrao2012@gmail.com [Air Glass Laboratory, Department of Physics, Shivaji University, Kolhapur 416 004, Maharashtra (India); Wagh, Pratap B.; Gupta, Satish C. [Applied Physics Division, Bhabha Atomic Research Centre (BARC), Trombay, Mumbai 400 085 (India)

    2010-03-01

    Control on the wettability of solid state materials is a classical and key issue in surface engineering. Optically transparent methyltriethoxysilane (MTES)-based silica films with water sliding angle as low as 9{sup o} were successfully prepared by two-step sol-gel co-precursor method. The emphasis is given to the effect of trimethylethoxysilane (TMES) as a co-precursor on water sliding behavior of silica films. The coating sol was prepared with molar ratio of methyltriethoxysilane (MTES), methanol (MeOH), acidic water (0.01 M, oxalic acid) and basic water (12 M, NH{sub 4}OH) kept constant at 1:12.73:3.58:3.58 respectively, and the molar ratio of TMES/MTES (M) was varied from 0 to 0.22. The static water contact angle as high as 120{sup o} and the water sliding angle as low as 9{sup o} was obtained by keeping the molar ratio (M) of TMES/MTES at 0.22. When the modified films were cured at temperature higher than 280 deg. C, the films became superhydrophilic. Further, the humidity study was carried out at a relative humidity of 90% at 30 deg. C over 60 days. We characterized the water repellent silica films by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), atomic force microscopy (AFM), % of optical transmission, humidity tests and static and dynamic water contact angle (CA) measurements.

  10. SYNTHESIS OF ZEOLITE SOCONY MOBIL FROM BLUE SILICA GEL AND RICE HUSK ASH AS CATALYSTS FOR HYDROTHERMAL LIQUEFACTION

    OpenAIRE

    SUYITNO; SANURYA PUTRI PURBANINGRUM; DOMINICUS DANARDONO; ALFAITORY EMHEMED SALEM; FATHI A. MANSUR

    2015-01-01

    Renewable biofuels produced by the hydrothermal liquefaction of rice husks have received much attention because of rapid increases in fuel consumption and corresponding declines in fossil fuel resources. To increase biofuel yields, template-free syntheses of Zeolite Socony Mobil (ZSM) catalysts based on blue silica gel and rice husk ash as silica sources were studied. After ZSM synthesis in a closed reactor at 170°C, the crystallinity and crystalline diameters of the products were determined ...

  11. Assembly of light-emitting diode based on hydrophilic CdTe quantum dots incorporating dehydrated silica gel.

    Science.gov (United States)

    Du, Jinhua; Wang, Chunlei; Xu, Xiaojing; Wang, Zhuyuan; Xu, Shuhong; Cui, Yiping

    2016-03-01

    Stable photoluminescence QD light-emitting diodes (QD-LEDs) were made based on hydrophilic CdTe quantum dots (QDs). A quantum dot-inorganic nanocomposite (hydrophilic CdTe QDs incorporating dehydrated silica gel) was prepared by two methods (rotary evaporation and freeze drying). Taking advantage of its viscosity, plasticity and transparency, dehydrated silica gel could be coated on the surface of ultraviolet (UV) light LEDs to make photoluminescence QD-LEDs. This new photoluminescence QD-LED, which is stable, environmentally non-toxic, easy to operate and low cost, could expand the applications of hydrophilic CdTe QDs in photoluminescence. Copyright © 2015 John Wiley & Sons, Ltd.

  12. Substrate integrated Lead-Carbon hybrid ultracapacitor with flooded, absorbent glass mat and silica-gel electrolyte configurations

    OpenAIRE

    Banerjee, A.; Ravikumar, MK; Jalajakshi, A; Kumar, Suresh P; Gaffoor, SA; Shukla, AK

    2012-01-01

    Lead-Carbon hybrid ultracapacitors (Pb-C HUCs) with flooded, absorbent-glass-mat (AGM) and silica-gel sulphuric acid electrolyte configurations are developed and performance tested. Pb-C HUCs comprise substrate-integrated PbO2 (SI-PbO2) as positive electrodes and high surface-area carbon with graphite-sheet substrate as negative electrodes. The electrode and silica-gel electrolyte materials are characterized by XRD, XPS, SEM, TEM, Rheometry, BET surface area, and FTIR spectroscopy in conjunct...

  13. Incorporation of mesoporous silica particles in gelatine gels: effect of particle type and surface modification on physical properties.

    Science.gov (United States)

    Pérez-Esteve, Édgar; Oliver, Laura; García, Laura; Nieuwland, Maaike; de Jongh, Harmen H J; Martínez-Máñez, Ramón; Barat, José Manuel

    2014-06-17

    The aim of this work was to investigate the impact of mesoporous silica particles (MSPs) on the physicochemical properties of filled protein gels. We have studied the effect of the addition of different mesoporous silica particles, either bare or functionalized with amines or carboxylates, on the physical properties of gelatine gels (5% w/v). Textural properties of the filled gels were investigated by uniaxial compression, while optical properties were investigated by turbidity. The MSPs were characterized with the objective of correlating particle features with their impact on the corresponding filled-gel properties. The addition of MSPs (both with and without functionalization) increased the stiffness of the gelatine gels. Furthermore, functionalized MSPs showed a remarkable increase in the strength of the gels and a slight reduction in the brittleness of the gels, in contrast with nonfunctionalized MSPs which showed no effect on these two properties. The turbidity of the gels was also affected by the addition of all tested MSPs, showing that the particles that formed smaller aggregates resulted in a higher contribution to turbidity. MSPs are promising candidates for the development of functional food containing smart delivery systems, also being able to modulate the functionality of protein gels.

  14. Thermal properties of wool fabric treated by phosphorus-doped silica sols through sol-gel method

    Directory of Open Access Journals (Sweden)

    Zhang Wei

    2014-01-01

    Full Text Available Wool fabric was treated with silica sol and phosphorus doped silica sol by sol-gel method in order to improve its thermal properties and flame retardance. The thermal stability, combustion behavior, and smoke suppression of the control and finished wool fabric were analyzed using thermogravimetric analysis, limited oxygen index, micro combustion calorimeter, and smoke chamber. The results showed that wool fabric treated by phosphorus doped silica sol had excellent thermal properties and flame retardance with higher final char residue and LOI value. Furthermore, heat release rate and smoke density results indicated the safety performance of the treated wool fabric on fire.

  15. Preparation and properties of aqueous castor oil-based polyurethane-silica nanocomposite dispersions through a sol-gel process.

    Science.gov (United States)

    Xia, Ying; Larock, Richard C

    2011-09-01

    Waterborne castor oil-based polyurethane-silica nanocomposites with the polymer matrix and silica nanoparticles chemically bonded have been successfully prepared through a sol-gel process. The formation of silica nanoparticles in water not only reinforces the resulting coatings, but also increases the crosslink density of the nanocomposites. The (29)Si solid state NMR spectrum indicates the formation of silica and the TEM indicates that the nanoparticles are embedded in the polymers, resembling a core-shell structure. The silica nanoparticles in the polymer matrix play an important role in improving both the mechanical properties and the thermal stabilities of the resulting nanocomposites. This work provides an effective and promising way to prepare biorenewable, high performance nanocomposite coatings.

  16. In situ synthesis of magnetic mesoporous silica via sol-gel process coupled with precipitation and oxidation

    Institute of Scientific and Technical Information of China (English)

    Junqi Zhao; Yujun Wang; Guangsheng Luo; Shenlin Zhu

    2011-01-01

    A novel method was proposed for the in situ synthesis of magnetite-containing mesoporous silica SBA-16 via a sol-gel process coupled with precipitation and oxidation. The effect of the added amounts of reactants on the mesostructural and magnetic properties of the magnetic mesoporous silica was investigated. It was determined that the synthesized magnetic mesoporous silica with a total pore volume of 0.64-0.96 cm3/g and an average pore diameter of 4.0-14.9 nm had a relatively high saturation magnetization value (1.11-5.77 emu/g) and a large surface area (258-747 m2/g). Lysozyme was chosen as a model protein to test the performance of the magnetic mesoporous silica as a protein adsorbent. The high adsorption capacity (up to 212 mg/g) suggested a promising future as bimolecular hosts for the magnetic mesoporous silica.

  17. Effect of chemically modified silicas on the properties of hybrid gel electrolyte for Li-ion batteries

    Science.gov (United States)

    Walkowiak, Mariusz; Zalewska, Aldona; Jesionowski, Teofil; Waszak, Daniel; Czajka, Bogdan

    The aim of the presented work was to perform a preliminary study the physico-chemical properties of hybrid organic-inorganic gel electrolytes for Li-ion batteries based on the PVdF-HFP polymeric matrix and surface modified fumed silicas. Modifications were done by means of the so-called dry method using seven different silanes differing in the nature of the principal functional group: N-2-(aminoethyl)-3-amino propyltrimethoxysilane, 3-glycidoxypropyltrimetoxysilane, 3-mercaptopropyltrimetoxysilane, n-octyltriethoxysilane, 3-(chloropropyl)trimethoxysilane, 3-methacryloxypropyltrimetoxysilane, vinyltrimethoxysilane. The PVdF-HFP gels were prepared according to the so-called Bellcore process (two-step method). Impact of the silicas surface functionality on the degree of crystallinity of the polymeric membranes was studied using the differential scanning calorimetry technique. Applicability of the prepared gel electrolytes for the Li-ion technology was estimated on the basis of specific conductivity measurements. It was shown that modification of the silica surface by most of the silanes causes an increase in the gel specific conductivity by about two orders of magnitude as compared to gel with unmodified silica.

  18. Effect of chemically modified silicas on the properties of hybrid gel electrolyte for Li-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Walkowiak, Mariusz; Waszak, Daniel; Czajka, Bogdan [Central Laboratory of Batteries and Cells, ul. Forteczna 12, 61-362 Poznan (Poland); Zalewska, Aldona [Warsaw University of Technology, Department of Chemistry, ul. Noakowskiego 3, 00-664 Warsaw (Poland); Jesionowski, Teofil [Poznan University of Technology, Institute of Chemical Technology and Engineering, Pl. Marii Sklodowskiej-Curie 2, 60-965 Poznan (Poland)

    2006-09-13

    The aim of the presented work was to perform a preliminary study the physico-chemical properties of hybrid organic-inorganic gel electrolytes for Li-ion batteries based on the PVdF-HFP polymeric matrix and surface modified fumed silicas. Modifications were done by means of the so-called dry method using seven different silanes differing in the nature of the principal functional group: N-2-(aminoethyl)-3-amino propyltrimethoxysilane, 3-glycidoxypropyltrimetoxysilane, 3-mercaptopropyltrimetoxysilane, n-octyltriethoxysilane, 3-(chloropropyl)trimethoxysilane, 3-methacryloxypropyltrimetoxysilane, vinyltrimethoxysilane. The PVdF-HFP gels were prepared according to the so-called Bellcore process (two-step method). Impact of the silicas surface functionality on the degree of crystallinity of the polymeric membranes was studied using the differential scanning calorimetry technique. Applicability of the prepared gel electrolytes for the Li-ion technology was estimated on the basis of specific conductivity measurements. It was shown that modification of the silica surface by most of the silanes causes an increase in the gel specific conductivity by about two orders of magnitude as compared to gel with unmodified silica. (author)

  19. Nanostructured Silica/Gold-Cellulose-Bonded Amino-POSS Hybrid Composite via Sol-Gel Process and Its Properties

    Science.gov (United States)

    Ramesh, Sivalingam; Kim, Heung Soo; Lee, Young-June; Hong, Gwang-Wook; Kim, Joo-Hyung

    2017-06-01

    It is demonstrated in this paper that silica nanoparticles coated with core/shell gold provide efficient thermal, optical, and morphological properties with respect to the cellulose-polyhedral oligomeric silsesquioxanes (POSS) hybrid system. The one-step synthesis of a silica/gold nanocomposite is achieved with a simultaneous hydrolysis and reduction of gold chloride in the presence of formic acid, and the trimethoxysilane group acts as a silica precursor. The focus here comprises the synthesis of cellulose-POSS and silica/gold hybrid nanocomposites using the following two methods: (1) an in situ sol-gel process and (2) a polyvinyl alcohol/tetrakis (hydroxymethyl)phosphonium chloride process. Accordingly, the silica/gold core/shell nanoparticles are synthesized. The growth and attachment of the gold nanoparticles onto the functionalized surface of the silica at the nanometer scale is achieved via both the sol-gel and the tetrakis (hydroxymethyl) phosphonium chloride processes. The cellulose-POSS-silica/gold nanocomposites are characterized according to Fourier transformed infrared spectroscopy, Raman, X-ray diffraction, UV, photoluminescence, SEM, energy-dispersive X-ray spectroscopy, TEM, thermogravimetric, and Brunauer-Emmett-Teller analyses.

  20. Alkynylation of aryl halides with perfluoro-tagged palladium nanoparticles immobilized on silica gel under aerobic, copper- and phosphine-free conditions in water.

    Science.gov (United States)

    Bernini, Roberta; Cacchi, Sandro; Fabrizi, Giancarlo; Forte, Giovanni; Petrucci, Francesco; Prastaro, Alessandro; Niembro, Sandra; Shafir, Alexandr; Vallribera, Adelina

    2009-06-07

    The utilization of perfluoro-tagged palladium nanoparticles immobilized on fluorous silica gel through fluorous-fluorous interactions (Pd(np)-/FSG) or linked to silica gel by covalent bonds (Pd(np)-) in the alkynylation of terminal alkynes with aryl halides under aerobic, copper- and phosphine-free conditions in water, and their recovery and re-utilization, is described.

  1. E ective Doping of Rare-earth Ionsin Silica Gel:A Novel Approach to Design Active Electronic Devices

    Institute of Scientific and Technical Information of China (English)

    D. Haranath∗; Savvi Mishra; Amish G. Joshi; Sonal Sahai; Virendra Shanker

    2011-01-01

    Eu3+luminescence spectroscopy has been used to investigate the effective doping of alkoxide-based silica (SiO2) gels using a novel pressure-assisted sol-gel method. Our results pertaining to intense photolumi-nescence (PL) from gel nanospheres can be directly attributed to the high specific surface area and remarkable decrease in unsaturated dangling bonds of the gel nanospheres under pressure. An increased dehydroxylation in an autoclave resulted in enhanced red (∼611 nm) PL emission from europium and is almost ten times brighter than the SiO2 gel made at atmospheric pressure and∼50℃ using conventional St¨ober-Fink-Bohn process. The presented results are entirely different from those reported earlier for SiO2:Eu3+ gel nanospheres and the origin of the enhanced PL have been discussed thoroughly.

  2. A biofriendly silica gel for in situ protein entrapment: biopolymer-assisted formation and its kinetic mechanism.

    Science.gov (United States)

    Wang, Guan-Hai; Zhang, Li-Ming

    2009-03-05

    In an attempt to develop a biofriendly sol-gel route for the rapid formation of biofunctional silica gels, a biopolymer with good biocompatibility was used to assist the gelation of glycol-modified tetraethoxysilane (GMT) in aqueous system without the addition of any organic solvents. It was found that the biopolymer used could act as an effective accelerator for the sol-gel transition of GMT and an increase of its amount could shorten greatly the gelation time. For such a gelation reaction, its apparent activation energy was determined to be 64.9 kJ/mol according to the Arrhenius equation. In particular, the kinetic mechanism for the formation of the silica gel was investigated by using dynamic theological data and a scaling fractal model. It was revealed that the biopolymer used could change the sol-gel transition mechanism from reaction-limited kinetics to diffusion-limited kinetics. Circular dichroism analyses confirmed the suitability of using the resultant silica gel for the in situ protein encapsulation.

  3. Organo-silica-titania nanocomposite elaborated by sol-gel processing with tunable optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Franc, J. [Laboratoire Traitement du Signal et Instrumentation, CNRS-UMR 5516, Universite Jean Monnet, 10 rue Barrouin, 42100 Saint-Etienne, 18 rue Benoit Lauras, F-42000 Saint-Etienne (France)]. E-mail: janyce.franc@univ-st-etienne.fr; Blanc, D. [Laboratoire Traitement du Signal et Instrumentation, CNRS-UMR 5516, Universite Jean Monnet, 10 rue Barrouin, 42100 Saint-Etienne, 18 rue Benoit Lauras, F-42000 Saint-Etienne (France); Zerroukhi, A. [Laboratoire de Rheologie des Matieres Plastiques, UMR CNRS 5156, 23 rue Paul Michelon, F-42023 Saint-Etienne Cedex 2 (France); Chalamet, Y. [Laboratoire de Rheologie des Matieres Plastiques, UMR CNRS 5156, 23 rue Paul Michelon, F-42023 Saint-Etienne Cedex 2 (France); Last, A. [Research Center Karlsruhe, Institute for Microstructure Technology, P.O. Box 3640, 76021 Karlsruhe (Germany); Destouches, N. [Laboratoire Traitement du Signal et Instrumentation, CNRS-UMR 5516, Universite Jean Monnet, 10 rue Barrouin, 42100 Saint-Etienne, 18 rue Benoit Lauras, F-42000 Saint-Etienne (France)

    2006-04-15

    Organically modified silica-titania thin films were elaborated by a sol-gel process and UV assisted photopolymerisation. Two different chelating agents, methacrylic acid (MAA) and a {beta}-diketone (2-(methacryloyloxy) ethyl acetoacetone (MAEA)) were compared in this work. It was demonstrated that the choice of the chelating agent is a key parameter to increase the molar ratio Si:Ti and therefore raise the refractive index of the material. {beta}-Diketone has proven to be a good candidate to stabilise the titanium precursor and its effects were compared to those observed with methacrylic acid. Fourier transform infrared spectroscopy was used to monitor the material formation and modification upon irradiation. M-lines spectroscopy was used to measure the refractive index of the material that varied between 1.51 and 1.59 depending on the titanium molar concentration. Optical properties were analysed in view of applications in the field of micro-optics and optical coatings.

  4. Silica-gel Catalyzed Facile Synthesis of 3,4-Dihydropyrimidinones

    Energy Technology Data Exchange (ETDEWEB)

    Agarwal, Sameer; Aware, Umesh; Patil, Amit; Rohera, Vinita; Jain, Mukul; Patel, Pankaj [Zydus Research Centre, Sarkhej-Bavla N.H., Ahmedabad (India); Ghate, Manjunath [Nirma University, Ahmedabad (India)

    2012-02-15

    We have developed a mild and highly effective procedure for the one-pot synthesis of substituted dihydropyrimidinones in high yields using silica gel as a green, highly efficient and recyclable heterogeneous catalyst. Our approach can be applied to the preparation of a wide range of synthetic analogues for structure-activity studies. Investigations in this direction are ongoing. The pyrimidinone ring is a basic substructure of numerous biologically active alkaloids and pharmaceutical products. These cores are regarded as one of the most important groups of drug-like scaffolds. 3,4-dihydropyrimidinones above are known to exhibit variety of pharmacological activity such as calcium channel modulation, mitotic kinesin Eg5 inhibition, antiviral, anti-inflammatory, antibacterial activity, etc.

  5. Study of optical properties of Macrophomina phaseolina impregnated sol-gel derived silica matrices.

    Science.gov (United States)

    Sharma, Sunita; Vandana; Ghoshal, S K; Arora, Pooja; Dilbaghi, Neeraj; Chaudhury, Ashok

    2009-11-01

    In the present frame of work, Macrophomina phaseolina is encapsulated in silica matrices at various concentrations by low temperature sol-gel technique using tetraethylorthosilicate (TEOS) as precursor. The optical and photophysical properties of these samples have been studied by second harmonics of Nd:YAG laser at 532 nm. UV-visible absorption spectra of samples have been recorded and it is found that the absorption increases with increase in concentration of fungus. Further, a decrease in output transmission intensity of the laser has been observed with increase in fungus concentration. The temporal response of these samples has also been examined. The results show that the fungus concentration can be measured within approximately 15-20 min. This method of optical sensing of fungus in test sample is faster than other techniques, such as the conventional colorimetric method which takes about 1 h.

  6. Theoretical study of simultaneous water and VOCs adsorption and desorption in a silica gel rotor

    DEFF Research Database (Denmark)

    Zhang, G.; Zhang, Y.F.; Fang, Lei

    2008-01-01

    One-dimensional partial differential equations were used to model the simultaneous water and VOC (Volatile Organic Compound) adsorption and desorption in a silica gel rotor which was recommended for indoor air cleaning. The interaction among VOCs and moisture in the adsorption and desorption...... by the temperatures of the rotor and the air stream. The VOC transfer equations were solved by discretizing them into explicit up-wind finite differential equations. The model was validated with experimental data. The calculated results suggested that the regeneration time designed for dehumidification may...... process was neglected in the model as the concentrations of VOC pollutants in typical indoor environment were much lower than that of moisture and the adsorbed VOCs occupied only a minor portion of adsorption capacity of the rotor. Consequently VOC transfer was coupled with heat and moisture transfer only...

  7. Hydrogen generation systems utilizing sodium silicide and sodium silica gel materials

    Science.gov (United States)

    Wallace, Andrew P.; Melack, John M.; Lefenfeld, Michael

    2015-07-14

    Systems, devices, and methods combine reactant materials and aqueous solutions to generate hydrogen. The reactant materials can sodium silicide or sodium silica gel. The hydrogen generation devices are used in fuels cells and other industrial applications. One system combines cooling, pumping, water storage, and other devices to sense and control reactions between reactant materials and aqueous solutions to generate hydrogen. Multiple inlets of varied placement geometries deliver aqueous solution to the reaction. The reactant materials and aqueous solution are churned to control the state of the reaction. The aqueous solution can be recycled and returned to the reaction. One system operates over a range of temperatures and pressures and includes a hydrogen separator, a heat removal mechanism, and state of reaction control devices. The systems, devices, and methods of generating hydrogen provide thermally stable solids, near-instant reaction with the aqueous solutions, and a non-toxic liquid by-product.

  8. The enhancement of benzotriazole on epoxy functionalized silica sol-gel coating for copper protection

    Science.gov (United States)

    Peng, Shusen; Zhao, Wenjie; Li, He; Zeng, Zhixiang; Xue, Qunji; Wu, Xuedong

    2013-07-01

    The influence of the amount of benzotriazole (BTA) on the wetting and anticorrosion ability of the epoxy functionalized silica sol-gel (ESol) coating was studied by various complementary methods. IR results demonstrate that BTA reacted with ESol through a 1:1 addition reaction of Nsbnd H to epoxy group. The water contact angle of the ESol coating increases with an increase in the amount of BTA. SEM and adhesion tests reveal that BTA could improve the adhesion of ESol to copper surface. Moreover, the best protection was achieved when the amount of BTA equals to the molar number of epoxy group in the ESol coating according to the results of electrochemical measurements and salt spray test.

  9. Textural characterization of silica gel from adsorption columns of the natural gas

    Energy Technology Data Exchange (ETDEWEB)

    Rockmann, Rico [Wilhelm Ostwald Inst. fuer Physikalische und Theoretische Chemie, Univ. Leipzig (Germany); Messow, Ulf [Univ. Leipzig (Germany); Kleinitz, Wolfram [Gaz de France Produktion Exploration Deutschland GmbH, Lingen (Ems) (Germany); Kalies, Grit [Inst. fuer Experimentelle Physik I, Univ. Leipzig (Germany)

    2008-12-15

    Commercial silica gel used in adsorption columns for the removal of natural gas liquids from a natural gas stream is analyzed in its textured parameters such as porosity, pore size distribution and surface area. The texture of the original material before application in adsorptions columns is compared with that of samples of material which had been in operation for almost seven years in natural gas adsorption columns. In order to obtain relevant structural information, different well-established experimental techniques are applied such as low-temperature adsorption volumetry, mercury intrusion and scanning electron microscopy. It is shown that experimental pore-size techniques are appropriate to characterize the adsorption capacity of a physical solvent and to obtain in this way information about the remaining efficiency of technical adsorber fillings. (orig.)

  10. Experimental research on dynamic operating characteristics of a novel silica gel-water adsorption chiller

    Institute of Scientific and Technical Information of China (English)

    WANG Dechang; WU Jingyi; WANG Ruzhu; DOU Weidong

    2007-01-01

    A novel silica gel-water adsorption chiller consisting of two adsorption/desorption chambers and an evaporator with one heat-pipe working chamber is experimentally studied.The dynamic operating characteristics of the chiller and the thermodynamic characteristics of the adsorber are obtained.The experimental results show that the dynamic operating characteristics of the chiller and the thermodynamic characteristics of the adsorber are satisfactory and that the cycle is a novel and effective adsorption cycle.A mass recovery process increases the cyclic adsorption capacity of the system and improves adaptability of the chiller to a lowgrade heat source.In addition,the experiment indicates that this novel chiller is highly suitable for an air conditioning system with a low dehumidification requirement or a system with a large cycle flowrate and an industrial cooling water system.

  11. Synthesis of mesoporous silica materials with ascorbic acid as template via sol-gel process

    Institute of Scientific and Technical Information of China (English)

    PANG, Jie-Bina; QIU, Kun- Yuan; WEI, Yen

    2000-01-01

    Mesoporous silica materials with pore diameters of 2-5 nm have been prepared using ascorbic acid as a nonsurfactant tem plate or pore-forming agent in HCl-catalyzed sol-gel reactions of tetraethylorthosilicate, followed by removing the ascorbic acid compound by extrraction with ethanol. Characteriztion results from nitrogen sorption isotherm, powder X-ray diffraction and transmission electron microscopy indicate that the materials have large specific surface areas ( e. g. 1000 m2/g) and pore vohmes ( e. g. 0.8 cm3/g). The mesoporosity is arisen from interconnecting disordered wormlike channels and pores with relatively broad size distributions. As the ascorbic acid concen tration is increased, the pore diameters and pore volumes of the materials increase.

  12. Study of Solar Driven Silica gel-Water based Adsorption Chiller

    Science.gov (United States)

    Habib, K.; Assadi, M. K.; Zainudin, M. H. B.

    2015-09-01

    In this study, a dynamic behaviour of a solar powered single stage four bed adsorption chiller has been analysed designed for Malaysian climate. Silica gel and water have been used as adsorbent-refrigerant pair. A simulation program has been developed for modeling and performance evaluation of the chiller using the meteorological data of Kuala Lumpur. The optimum cooling capacity and coefficient of performance (COP) are calculated in terms of adsorption/desorption cycle time and regeneration temperature. Results indicate that the chiller is feasible even when low temperature heat source is available. Results also show that the adsorption cycle can achieve a cooling capacity of 14 kW when the heat source temperature is about 85°C.

  13. Analysis based on the diffusion model for saturation silica gel with water vapor at conservation units steam circuit TPP

    Science.gov (United States)

    Goldaev, Sergey; Khushvaktov, Alisher

    2015-01-01

    A quantitative analysis of the diffusion model dehumidifying air in the steam circuit of TPP, with a layer of silica gel. Showed that such an approximation, supplemented the experimental value of the coefficient of free diffusion identified by the developed method gives reliable values for the concentration of water vapor absorption over time.

  14. Processing of CuAlMn Shape Memory Foams with Open Spherical Pores by Silica-Gel Beads Infiltration Method

    Science.gov (United States)

    Li, Hua; Yuan, Bin; Gao, Yan

    2016-10-01

    A molten metal infiltration process with amorphous SiO2 (silica-gel) beads as space holders was used to prepare Cu-based shape memory foams in this article. We found that the silica-gel beads with micropores inside expanded when being heated to elevated temperatures and that proper control of the expansion of silica-gel beads helped form necks between the beads with different bonding extent, which had been taken advantage of to have a good control of the foam morphology and porosity, by carefully designing suitable procedures and choosing proper parameters for the process. In addition, we studied in detail the effect of heating temperature, silica-gel bead density, and infiltration pressure of the present process on the morphology and porosity of CuAlMn shape memory foams. By coordinating these three key parameters, CuAlMn shape memory foams with open spherical pores and adjustable porosity from 66 to 85 pct were reliably produced.

  15. Sol–gel one-pot synthesis in soft conditions of mesoporous silica materials ready for drug delivery system

    NARCIS (Netherlands)

    Tourne-Peteilh, C.; Begu, S.; Lerner, D.A.; Galarneau, A.; Lafont, U.; Devoiselle, J.-M.

    2011-01-01

    The present work reveals a new and simple strategy, a one-step sol–gel procedure, to encapsulate a low water-soluble drug in silica mesostructured microparticles and to improve its release in physiological media. The synthesis of these new materials is based on the efficient solubilisation of a poor

  16. Synthetic aspects and characterization of polypropylene–silica nanocomposites prepared via solid-state modification and sol–gel reactions

    NARCIS (Netherlands)

    Jain, Sachin; Goossens, Han; Picchioni, Francesco; Magusin, Pieter; Mezari, Brahim; Duin, Martin van

    2005-01-01

    A new route is developed by combining solid-state modification (SSM) by grafting vinyl triethoxysilane (VTES) with a sol–gel method to prepare PP/silica nanocomposites with varying degree of adhesion between filler and matrix. VTES was grafted via SSM in porous PP particles. Bulk polymerization unde

  17. Iodine Supported on 3-Aminopropyl Silica Gel as Efficient Catalyst for Acetylation of Alcohols under Solvent-free Conditions

    Institute of Scientific and Technical Information of China (English)

    MAHDAVI Hossein; GHAEMY Mosa; ZERAATPISHEH Fatemeh

    2009-01-01

    3-Aminopropyl silica gel (I2/APSG) was found to catalyze the acetylation of alcohols and phenols efficiently with acetic anhydride. The reaction is mild and selective with high yields. A wide variety of alcohols and phenols are selectively converted into the corresponding acetates using I2/APSG under solvent-free conditions at room tem-perature.

  18. Sol–gel one-pot synthesis in soft conditions of mesoporous silica materials ready for drug delivery system

    NARCIS (Netherlands)

    Tourne-Peteilh, C.; Begu, S.; Lerner, D.A.; Galarneau, A.; Lafont, U.; Devoiselle, J.-M.

    2011-01-01

    The present work reveals a new and simple strategy, a one-step sol–gel procedure, to encapsulate a low water-soluble drug in silica mesostructured microparticles and to improve its release in physiological media. The synthesis of these new materials is based on the efficient solubilisation of a poor

  19. Synthetic aspects and characterization of polypropylene-silica nanocomposites prepared via solid-state modification and sol-gel reactions

    NARCIS (Netherlands)

    Jain, S; Goossens, H; Picchioni, F; Magusin, P; Mezari, B

    2005-01-01

    A new route is developed by combining solid-state modification (SSM) by grafting vinyl triethoxysilane (VTES) with a sol-gel method to prepare PP/silica nanocomposites with varying degree of adhesion between filler and matrix. VTES was grafted via SSM in porous PP particles. Bulk polymerization unde

  20. Comparison of the surface ion density of silica gel evaluated via spectral induced polarization versus acid-base titration

    Science.gov (United States)

    Hao, Na; Moysey, Stephen M. J.; Powell, Brian A.; Ntarlagiannis, Dimitrios

    2016-12-01

    Surface complexation models are widely used with batch adsorption experiments to characterize and predict surface geochemical processes in porous media. In contrast, the spectral induced polarization (SIP) method has recently been used to non-invasively monitor in situ subsurface chemical reactions in porous media, such as ion adsorption processes on mineral surfaces. Here we compare these tools for investigating surface site density changes during pH-dependent sodium adsorption on a silica gel. Continuous SIP measurements were conducted using a lab scale column packed with silica gel. A constant inflow of 0.05 M NaCl solution was introduced to the column while the influent pH was changed from 7.0 to 10.0 over the course of the experiment. The SIP measurements indicate that the pH change caused a 38.49 ± 0.30 μS cm- 1 increase in the imaginary conductivity of the silica gel. This increase is thought to result from deprotonation of silanol groups on the silica gel surface caused by the rise in pH, followed by sorption of Na+ cations. Fitting the SIP data using the mechanistic model of Leroy et al. (Leroyet al., 2008), which is based on the triple layer model of a mineral surface, we estimated an increase in the silica gel surface site density of 26.9 × 1016 sites m- 2. We independently used a potentiometric acid-base titration data for the silica gel to calibrate the triple layer model using the software FITEQL and observed a total increase in the surface site density for sodium sorption of 11.2 × 1016 sites m- 2, which is approximately 2.4 times smaller than the value estimated using the SIP model. By simulating the SIP response based on the calibrated surface complexation model, we found a moderate association between the measured and estimated imaginary conductivity (R2 = 0.65). These results suggest that the surface complexation model used here does not capture all mechanisms contributing to polarization of the silica gel captured by the SIP data.

  1. Application of Hectorite-Coated Silica Gel Particles as a Packing Material for Chromatographic Resolution.

    Science.gov (United States)

    Okada, Tomohiko; Kumasaki, Aisaku; Shimizu, Kei; Yamagishi, Akihiko; Sato, Hisako

    2016-08-01

    A new type of clay column particles was prepared, in which a hectorite layer (∼0.1 µm thickness) covered uniformly the surface of amorphous silica particles with an average radius of 5 µm (ref. Okada et al., The Journal of Physical Chemistry C, 116, 21864-21869 (2012)). The hectorite layer was fully ion-exchanged with Δ-[Ru(phen)3](2+) (phen = 1,10-phenanthroline) ions by being immersed in a methanol solution of Δ-[Ru(phen)3](ClO4)2 (1 mM). The modified silica gel particles thus prepared were packed into a stainless steel tube (4 mm (i.d.) × 25 cm) as a high-performance liquid chromatography column. Optical resolution was achieved when the racemic mixtures of several metal complexes or organic molecules were eluted with methanol. In the case of tris(acetylacetonato)ruthenium(III) ([Ru(acac)3]), for example, the Λ- and Δ-enantiomers gave an elution volume of 2.6 and 3.0 mL, respectively, with the separation factor of 1.2. The total elution volume (5 mL) was nearly one-tenth for the previously reported column of the same size (RU-1 (Shiseido Co., Ltd.)) packed with the spray-dried particles of synthetic hectorite (average radius 5 µm) ion-exchanged by the same Ru(II) complexes.

  2. Comparison of nanoparticle exposures between fumed and sol-gel nano-silica manufacturing facilities.

    Science.gov (United States)

    Oh, Sewan; Kim, Boowook; Kim, Hyunwook

    2014-01-01

    Silica nanoparticles (SNPs) are widely used all around the world and it is necessary to evaluate appropriate risk management measures. An initial step in this process is to assess worker exposures in their current situation. The objective of this study was to compare concentrations and morphologic characteristics of fumed (FS) and sol-gel silica nanoparticles (SS) in two manufacturing facilities. The number concentration (NC) and particle size were measured by a real-time instrument. Airborne nanoparticles were subsequently analyzed using a TEM/EDS. SNPs were discharged into the air only during the packing process, which was the last manufacturing step in both the manufacturing facilities studied. In the FS packing process, the geometric mean (GM) NC in the personal samples was 57,000 particles/cm(3). The geometric mean diameter (GMD) measured by the SMPS was 64 nm. Due to the high-temperature formation process, the particles exhibited a sintering coagulation. In the SS packing process that includes a manual jet mill operation, the GM NC was calculated to be 72,000 particles/cm(3) with an assumption of 1,000,000 particles/cm(3) when the upper limit is exceeded (5% of total measure). The particles from SS process had a spherical-shaped morphology with GMD measured by SMPS of 94 nm.

  3. Size-selective recognition of catecholamines by molecular imprinting on silica-alumina gel.

    Science.gov (United States)

    Ling, Tzong-Rong; Syu, Yau Zen; Tasi, Yau-Ching; Chou, Tse-Chuan; Liu, Chung-Chiun

    2005-12-15

    The preparation of a catecholamine receptor was carried out using a molecular imprinting method with silica-alumina gel to form complementary structures for template recognition. The molecularly imprinted polymer (MIP) was synthesized by the condensation of silicate from tetraethyl orthosilictate (TEOS) under hydrothermal conditions at 60 degrees C. Aluminum chloride was added as a functional monomer to increase the material's rebinding ability. The selectivity of the MIP receptor prepared with different ratios of template to Si and Al, was examined with seven analytes including: dopamine, epinephrine, norepinephrine, ascorbic acid, homovanillic acid, uric acid, and l-tyrosine. The results showed a size selective effect for the receptors with respect to the recognition of the catecholamines. Some factors affecting the recognition ability were investigated including: the solution pH of analytes, surface capping on the MIP, and the imprinting pH of the silica-alumina solution. Also, the catecholamine MIP films on quartz crystal microbalance (QCM) electrodes were fabricated as sensors for in situ monitoring of the analytes in a 2-propanol solution.

  4. SOL-GEL SILICA-BASED Ag–Ca–P COATINGS WITH AGRESSIVE PRETREATMENT OF TITANIUM SUBSTRATE

    Directory of Open Access Journals (Sweden)

    ELENA BORSHCHEVA

    2011-12-01

    Full Text Available The aim of the experiment was the obtaining of thin silica coatings on titanium by sol-gel method, using mechanical (SiC - paper No.180 and chemical (leaching in HF pretreatments of the titanium substrates. The solutions were based on TEOS. For the sol-gel dipping process 4 different solutions were prepared: silica, silica with AgNO3 and silica + AgNO3 with brushite (CaHPO4·2H2O or monetite (CaHPO4 powders. The solutions were aged for 7 and 14 days at laboratory temperature. After sol-gel dip-coating process the samples were dried and fired. The adhesion of fired coatings was measured by tape test according to ASTM procedure and the bioactivity of the coatings was tested using in vitro test. The surfaces of the samples after firing, tape test and in vitro test were observed with the optical and electron microscopes. The firing results showed that silica-silver coatings did not change, brushite sol-gel coatings have cracked and the monetite sol-gel coatings have cracked also, but less than brushite ones. In spite of coating´s crackings, the square’s frames made on the surfaces were without any breakdowns after tape tests and the adhesion of all coatings was very good, classified by the highest grade 5. The results of in vitro tests showed that all coatings interacted with simulated body fluid (SBF. After exposition in SBF the new layer formed on substrates. In case of 7 days aged coatings containing brushite the new layer was uniform and compact. In case of 7 days aged coatings containing monetite the new layer was formed by crystals aggregated tightly together. The monetite and brushite coatings prepared from 14 days aged sol were the same as previous ones, but they were thicker. X-ray analyses after in vitro test confirmed dellaite, titanate and hydroxyapatite phases.

  5. Potentiometric detection of silver (I) ion based on carbon paste electrode modified with diazo-thiophenol-functionalized nanoporous silica gel

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Ting; Chai Yaqin, E-mail: yqchai@swu.edu.cn; Yuan Ruo; Guo Junxiang

    2012-07-01

    For the first time, triazene compound functionalized silica gel was incorporated into carbon paste electrode for the potentiometric detection of silver (I) ion. A novel diazo-thiophenol-functionalized silica gel (DTPSG) was synthesized, and the presence of DTPSG acted as not only a paste binder, but also a reactive material. The electrode with optimum composition, exhibited an excellent Nernstian response to Ag{sup +} ion ranging from 1.0 Multiplication-Sign 10{sup -6} to 1.0 Multiplication-Sign 10{sup -1} M with a detection limit of 9.5 Multiplication-Sign 10{sup -7} M and a slope of 60.4 {+-} 0.2 mV dec{sup -1} over a wide pH range (4.0-9.0) with a fast response time (50 s) at 25 Degree-Sign C. The electrode also showed a long-time stability, high selectivity and reproducibility. The response mechanism of the proposed electrode was investigated by using AC impedance. Moreover, the electrode was successfully applied for the determination of silver ions in radiology films, and for potentiometric titration of the mixture solution of Cl{sup -} and Br{sup -} ions. - Highlights: Black-Right-Pointing-Pointer Functionalized silica gels have become promising materials. Black-Right-Pointing-Pointer This work is the first attempt to apply triazene functionalized silica gel. Black-Right-Pointing-Pointer The Functionalized silica gels were used to detect silver. Black-Right-Pointing-Pointer The response of the previously reported papers are compared with this work. Black-Right-Pointing-Pointer The result indicates the proposed electrode is better than reported Ag{sup +} electrodes.

  6. Specific Interactions of Neutral Side Chains of an Adsorbed Protein with the Surface of α-Quartz and Silica Gel.

    Science.gov (United States)

    Odinokov, Alexey V; Bagaturyants, Alexander A

    2015-07-16

    Many key features of the protein adsorption on the silica surfaces still remain unraveled. One of the open questions is the interaction of nonpolar side chains with siloxane cavities. Here, we use nonequilibrium molecular dynamics simulations for the detailed investigation of the binding of several hydrophobic and amphiphilic protein side chains with silica surface. These interactions were found to be a possible driving force for protein adsorption. The free energy gain was larger for the disordered surface of amorphous silica gel as compared to α-quartz, but the impact depended on the type of amino acid. The dependence was analyzed from the structural point of view. For every amino acid an enthalpy-entropy compensation behavior was observed. These results confirm a hypothesis of an essential role of hydrophobic interactions in protein unfolding and irreversible adsorption on the silica surface.

  7. Silica sol-gel encapsulated methylotrophic yeast as filling of biofilters for the removal of methanol from industrial wastewater.

    Science.gov (United States)

    Kamanina, Olga A; Lavrova, Daria G; Arlyapov, Viacheslav A; Alferov, Valeriy A; Ponamoreva, Olga N

    2016-10-01

    This research suggests the use of new hybrid biomaterials based on methylotrophic yeast cells covered by an alkyl-modified silica shell as biocatalysts. The hybrid biomaterials are produced by sol-gel chemistry from silane precursors. The shell protects microbial cells from harmful effects of acidic environment. Potential use of the hybrid biomaterials based on methylotrophic yeast Ogataea polymorpha VKM Y-2559 encapsulated into alkyl-modified silica matrix for biofilters is represented for the first time. Organo-silica shells covering yeast cells effectively protect them from exposure to harmful factors, including extreme values of pH. The biofilter based on the organic silica matrix encapsulated in the methylotrophic yeast Ogataea polymorpha BKM Y-2559 has an oxidizing power of 3 times more than the capacity of the aeration tanks used at the chemical plants during methyl alcohol production. This may lead to the development of new and effective industrial wastewater treatment technologies.

  8. Structure and dynamics of spin-labeled insulin entrapped in a silica matrix by the sol-gel method.

    Science.gov (United States)

    Vanea, E; Gruian, C; Rickert, C; Steinhoff, H-J; Simon, V

    2013-08-12

    The structure and conformational dynamics of insulin entrapped into a silica matrix was monitored during the sol to maturated-gel transition by electron paramagnetic resonance (EPR) spectroscopy. Insulin was successfully spin-labeled with iodoacetamide and the bifunctional nitroxide reagent HO-1944. Room temperature continuous wave (cw) EPR spectra of insulin were recorded to assess the mobility of the attached spin labels. Insulin conformation and its distribution within the silica matrix were studied using double electron-electron resonance (DEER) and low-temperature cw-EPR. A porous oxide matrix seems to form around insulin molecules with pore diameters in the order of a few nanometers. Secondary structure of the encapsulated insulin investigated by Fourier transform infrared spectroscopy proved a high structural integrity of insulin even in the dried silica matrix. The results show that silica encapsulation can be used as a powerful tool to effectively isolate and functionally preserve biomolecules during preparation, storage, and release.

  9. In Vivo skin hydration and anti-erythema effects of Aloe vera, Aloe ferox and Aloe marlothii gel materials after single and multiple applications

    Science.gov (United States)

    Fox, Lizelle T.; du Plessis, Jeanetta; Gerber, Minja; van Zyl, Sterna; Boneschans, Banie; Hamman, Josias H.

    2014-01-01

    Objective: To investigate the skin hydrating and anti-erythema activity of gel materials from Aloe marlothii A. Berger and A. ferox Mill. in comparison to that of Aloe barbadensis Miller (Aloe vera) in healthy human volunteers. Materials and Methods: Aqueous solutions of the polisaccharidic fractions of the selected aloe leaf gel materials were applied to the volar forearm skin of female subjects. The hydration effect of the aloe gel materials were measured with a Corneometer® CM 825, Visioscan® VC 98 and Cutometer® dual MPA 580 after single and multiple applications. The Mexameter® MX 18 was used to determine the anti-erythema effects of the aloe material solutions on irritated skin areas. Results: The A. vera and A. marlothii gel materials hydrated the skin after a single application, whereas the A. ferox gel material showed dehydration effects compared to the placebo. After multiple applications all the aloe materials exhibited dehydration effects on the skin. Mexameter® readings showed that A. vera and A. ferox have anti-erythema activity similar to that of the positive control group (i.e. hydrocortisone gel) after 6 days of treatment. Conclusion: The polysaccharide component of the gel materials from selected aloe species has a dehydrating effect on the skin after multiple applications. Both A. vera and A. ferox gel materials showed potential to reduce erythema on the skin similar to that of hydrocortisone gel. PMID:24991119

  10. Phospholipid Fatty Acids as Physiological Indicators of Paracoccus denitrificans Encapsulated in Silica Sol-Gel Hydrogels

    Directory of Open Access Journals (Sweden)

    Josef Trögl

    2015-02-01

    Full Text Available The phospholipid fatty acid (PLFA content was determined in samples of Paracoccus denitrificans encapsulated in silica hydrogel films prepared from prepolymerized tetramethoxysilane (TMOS. Immediately after encapsulation the total PLFA concentration was linearly proportional to the optical density (600 nm of the input microbial suspension (R2 = 0.99. After 7 days this relationship remained linear, but with significantly decreased slope, indicating a higher extinction of bacteria in suspensions of input concentration 108 cells/mL and higher. trans-Fatty acids, indicators of cytoplasmatic membrane disturbances, were below the detection limit. The cy/pre ratio (i.e., ratio of cyclopropylated fatty acids (cy17:0 + cy19:0 to their metabolic precursors (16:1ω7 + 18:1ω7, an indicator of the transition of the culture to a stationary growth-phase, decreased depending on co-immobilization of nutrients in the order phosphate buffer > mineral medium > Luria Broth rich medium. The ratio, too, was logarithmically proportional to cell concentration. These results confirm the applicability of total PLFA as an indicator for the determination of living biomass and cy/pre ratio for determination of nutrient limitation of microorganisms encapsulated in sol-gel matrices. This may be of interest for monitoring of sol-gel encapsulated bacteria proposed as optical recognition elements in biosensor construction, as well as other biotechnological applications.

  11. Colloidal quantum-dot-based silica gel glass: two-photon absorption, emission, and quenching mechanism.

    Science.gov (United States)

    Li, Jingzhou; Dong, Hongxing; Zhang, Saifeng; Ma, Yunfei; Wang, Jun; Zhang, Long

    2016-09-28

    Two-photon (TP) three-dimensional solid matrices have potential applications in high density optical data reading and storage, infrared-pumped visible displays, lasers, etc. Such technologies will benefit greatly from the advantageous properties of TP materials including tunable emission wavelength, photostability, and simple chemical processing. Here, this ideal TP solid is made possible by using a facile sol-gel process to engineer colloid quantum dots into silica gel glass. Characterization using an open-aperture Z-scan technique shows that the solid matrices exhibited significant TP optical properties with a TP absorption coefficient of (9.41 ± 0.39) × 10(-2) cm GW(-1) and a third-order nonlinear figure of merit of (7.30 ± 0.30) × 10(-14) esu cm. In addition, the dependence of the TP properties on high-temperature thermal treatment is studied in detail to obtain a clear insight for practical applications. The results illustrate that the sample can maintain stable TP performance below the synthesis temperature of the CdTe/CdS colloidal quantum dots. Furthermore, the mechanisms for thermal quenching of photoluminescence under different temperature regimes are clarified as a function of the composition.

  12. Reaction parameter study for the chemical synthesis of adsorbent silica gel

    Directory of Open Access Journals (Sweden)

    María Carolina Sáenz

    2010-07-01

    Full Text Available This article presents an appropriate set of reaction parameters (reaction temperature, sulphuric acid and sodium silicate reagent concentration for obtaining adsorbent silica gel (ASG using Colombian-produced raw materials. The core of ASG synthesis lies in sulphuric acid’s neutralisation reaction with sodium silicate. Their effect on final ASG moisture adsorption capacity was measured after changing such synthesis’ above–mentioned reaction parameters. Within the range of conditions studied, it was found that the highest adsorption capacity occurred by combining both low sodium silicate concentration with high temperatures or high sulphuric acid concentration and temperature. Synthesised ASG was also compared to a commercial product (Gel de sílice granulare con indicatore. Montedison group. Batch number 1684G100. Code number 453301 using adsorption capacity plots, BET areas, X–ray di-ffraction, mass and infrared spectrometry and mechanical strength measurements. Synthesised ASG presented larger specific surface areas but weaker mechanical strength than the commercial one. Likewise, all evaluated samples exhibited a low degree of molecular arrangement and conventional ASG chemical structure.

  13. MECHANISMS CONTROLLING Ca ION RELEASE FROM SOL-GEL DERIVED IN SITU APATITE-SILICA NANOCOMPOSITE POWDER

    Directory of Open Access Journals (Sweden)

    Seyed Mohsen Latifi

    2015-03-01

    Full Text Available Ca ion release from bioactive biomaterials could play an important role in their bioactivity and osteoconductivity properties. In order to improve hydroxyapatite (HA dissolution rate, in situ apatite-silica nanocomposite powders with various silica contents were synthesized via sol-gel method and mechanisms controlling the Ca ion release from them were investigated. Obtained powders were characterized by X-ray diffraction (XRD and transmission electron spectroscopy (TEM techniques, acid dissolution test, and spectroscopy by atomic absorption spectrometer (AAS. Results indicated the possible incorporation of (SiO44- into the HA structure and tendency of amorphous silica to cover the surface of HA particles. However, 20 wt. % silica was the lowest amount that fully covered HA particles. All of the nanocomposite powders showed more Ca ion release compared with pure HA, and HA - 10 wt. % silica had the highest Ca ion release. The crystallinity, the crystallite size, and the content of HA, along with the integrity, thickness, and ion diffusion possibility through the amorphous silica layer on the surface of HA, were factors that varied due to changes in the silica content and were affected the Ca ion release from nanocomposite powders.

  14. Sol-Gel-Based Titania-Silica Thin Film Overlay for Long Period Fiber Grating-Based Biosensors.

    Science.gov (United States)

    Chiavaioli, Francesco; Biswas, Palas; Trono, Cosimo; Jana, Sunirmal; Bandyopadhyay, Somnath; Basumallick, Nandini; Giannetti, Ambra; Tombelli, Sara; Bera, Susanta; Mallick, Aparajita; Baldini, Francesco

    2015-12-15

    An evanescent wave optical fiber biosensor based on titania-silica-coated long period grating (LPG) is presented. The chemical overlay, which increases the refractive index (RI) sensitivity of the sensor, consists of a sol-gel-based titania-silica thin film, deposited along the sensing portion of the fiber by means of the dip-coating technique. Changing both the sol viscosity and the withdrawal speed during the dip-coating made it possible to adjust the thickness of the film overlay, which is a crucial parameter for the sensor performance. After the functionalization of the fiber surface using a methacrylic acid/methacrylate copolymer, an antibody/antigen (IgG/anti-IgG) assay was carried out to assess the performance of sol-gel based titania-silica-coated LPGs as biosensors. The analyte concentration was determined from the wavelength shift at the end of the binding process and from the initial binding rate. This is the first time that a sol-gel based titania-silica-coated LPG is proposed as an effective and feasible label-free biosensor. The specificity of the sensor was validated by performing the same model assay after spiking anti-IgG into human serum. With this structured LPG, detection limits of the order of tens of micrograms per liter (10(-11) M) are attained.

  15. The Mechanism of Pseudomorphic Transformation of Spherical Silica Gel into MCM-41 Studied by PFG NMR Diffusometry

    Directory of Open Access Journals (Sweden)

    Roger Gläser

    2013-08-01

    Full Text Available The pseudomorphic transformation of spherical silica gel (LiChrospher® Si 60 into MCM-41 was achieved by treatment at 383 K for 24 h with an aqueous solution of cetyltrimethylammonium hydroxide (CTAOH instead of hexadecyltrimethylammonium bromide (CTABr and NaOH. The degree of transformation was varied via the ratio of CTAOH solution to initial silica gel rather than synthesis duration. The transformed samples were characterized by N2 sorption at 77 K, mercury intrusion porosimetry, X-ray diffraction (XRD and scanning electron microscopy (SEM. Thus, MCM-41 spheres with diameters of ca. 12 μm, surface areas >1000 m2 g−1, pore volumes >1 cm3 g−1 and a sharp pore width distribution, adjustable between 3.2 and 4.5 nm, were obtained. A thorough pulsed field gradient nuclear magnetic resonance (PFG NMR study shows that the diffusivity of n-heptane confined in the pores of the solids passes through a minimum with progressing transformation. The final product of pseudomorphic transformation to MCM-41 does not exhibit improved transport properties compared to the initial silica gel. Moreover, the PFG NMR results support that the transformation occurs via formation and subsequent growth of domains of <1 μm containing MCM-41 homogeneously distributed over the volume of the silica spheres.

  16. Determination of arsenate in water by anion selective membrane electrode using polyurethane–silica gel fibrous anion exchanger composite

    Energy Technology Data Exchange (ETDEWEB)

    Khan, Asif Ali, E-mail: asifkhan42003@yahoo.com; Shaheen, Shakeeba, E-mail: shakeebashaheen@ymail.com

    2014-01-15

    Highlights: • PU–Si gel is new anion exchanger material synthesized and characterized. • This material used as anion exchange membrane is applied for electroanalytical studies. • The method for detection and determination of AsO{sub 4}{sup 3−} in traces amounts discussed. • The results are also verified from arsenic analyzer. -- Abstract: Polyurethane (PU)–silica (Si gel) based fibrous anion exchanger composites were prepared by solid–gel polymerization of polyurethane in the presence of different amounts of silica gel. The formation of PU–Si gel fibrous anion exchanger composite was characterized by Fourier transform infra-red spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA-DTA), scanning electron microscopy (SEM) and elemental analysis. The membrane having a composition of 5:3 (PU:Si gel) shows best results for water content, porosity, thickness and swelling. Our studies show that the present ion selective membrane electrode is selective for arsenic, having detection limit (1 × 10{sup −8} M to 1 × 10{sup −1} M), response time (45 s) and working pH range (5–8). The selectivity coefficient values for interfering ions indicate good selectivity for arsenate (AsO{sub 4}{sup 3−}) over interfering anions. The accuracy of the detection limit results was compared by PCA-Arsenomat.

  17. Preparation of 4-butylaniline-bonded silica gel for the solid-phase extraction of flavone glycosides.

    Science.gov (United States)

    Chu, Ganghui; Cai, Wensheng; Shao, Xueguang

    2015-04-01

    To extract flavone glycosides efficiently, a new extraction material based on 4-butylaniline-bonded silica gel was prepared using a two-step grafting method including a ring-opening reaction and synchronous hydrolysis. Preparation of the silica-based material was easily achieved under mild conditions, and the material was characterized by Fourier transform infrared spectroscopy, elemental analysis, and scanning electron microscopy. The material was used in solid-phase extraction, and the extraction can be performed in neutral conditions without regard to ionic strength. Selectivity tests of 14 compounds on the extraction cartridge showed that the material has a high affinity to flavone glycosides in contrast to octadecyl silica, and the extraction yields for four flavone glycosides were found to be >93%. Selectivity tests further reveal that the adsorption on its surface is likely attributed to multiple interactions, including hydrophobic interactions, π-π interactions, and hydrogen bonding. To explore the applicability of 4-butylaniline-bonded silica gel, naringin and hesperidin from Simotang oral liquid were extracted, and the extraction yields were >90%, which is distinguished from silica cartridge.

  18. A BIDISPERSE MODEL TO STUDY THE HYDROLYSIS OF MALTOSE USING GLUCOAMYLASE IMMOBILIZED IN SILICA AND WRAPPED IN PECTIN GEL

    Directory of Open Access Journals (Sweden)

    L.R.B. Gonçalves

    1997-12-01

    Full Text Available In this work, a bidisperse model is built to represent the hydrolysis of maltose using immobilized glucoamylase. The experimental set is a mixed-batch reactor, maintained at 30ºC, with pectin gel spherical particles that contain enzyme immobilized in macroporous silica. The possibility of substrate adsorption on the pectin gel is also studied because this phenomenon may result in smaller values of diffusivity. Equilibrium assays are then performed for different substrates (maltose, lactose and glucose at different temperatures and pHs. These assays show that adsorption on the pectin gel is not important for the three dextrins analysed. The bidisperse model presents a good fit with the experimental data, when using previously-estimated kinetic and mass transfer parameters (Gonçalves et al., 1997. This result shows that the methodology used (wrapping the silica in pectin gel is appropriate for experimental studies with silica, since it allows a higher degree of agitation without causing shearing

  19. Insecticidal efficacy of silica gel with Juniperus oxycedrus ssp. oxycedrus (Pinales: Cupressaceae) essential oil against Sitophilus oryzae (Coleoptera: Curculionidae) and Tribolium confusum (Coleoptera: Tenebrionidae).

    Science.gov (United States)

    Athanassiou, Christos G; Kavallieratos, Nickolas C; Evergetis, Epameinondas; Katsoula, Anna-Maria; Haroutounian, Serkos A

    2013-08-01

    Laboratory bioassays were carried out to evaluate the effect of silica gel enhanced with the essential oil (EO) of Juniperus oxycedrus L. ssp. oxycedrus (Pinales: Cupressaceae) (derived from berry specimens from Greece) against adults of Sitophilus oryzae (L.) (Coleoptera: Curculionidae) and Tribolium confusum Jacquelin du Val (Coleoptera: Tenebrionidae). For that purpose, a dry mixture consisting of 500 mg of silica gel that had absorbed 2.18 mg of EO (total weight: 502.18 mg) was tested at three doses; 0.125, 0.250, and 0.5 g/kg of wheat, corresponding to 125, 250, and 500 ppm, respectively, and silica gel alone at 0.5 g/kg of wheat corresponding to 500 ppm, at different exposure intervals (24 and 48 h and 7 and 14 d for S. oryzae; 24 and 48 h and 7, 14, and 21 d for T. confusum). The chemical content of the specific EO was determined by gas chromatography (GC)-mass spectrometry (MS) analyses indicating the presence of 31 constituents with myrcene and germacrene-D being the predominant compounds. The bioactivity results for S. oryzae indicated that 48 h of exposure in wheat resulted in an 82% mortality for treatment with 500 ppm of the enhanced silica gel. For 7 d of exposure, 100 and 98% of S. oryzae adults died when they were treated with 500 and 250 ppm of enhanced silica gel, respectively. At 14 d of exposure, all adults died both at 250 and 500 ppm of enhanced silica gel. At 48 h, 7 and 14 d of exposure significantly less S. oryzae adults died in wheat treated with silica gel alone than at 250 or 500 ppm of enhanced silica gel. In the case of T. confusum, at 7 d of exposure, mortality in wheat treated with silica gel only was significantly higher in comparison to the other treatments. At the 14 d of exposure mortality in wheat treated with 500 ppm of silica gel alone was significantly higher than 125 and 250 ppm of the enhanced silica gel. Similar trends were also noted at 21 d of exposure, indicating that there is no enhancement effect from the addition of

  20. Thermal Stability and Luminescence Properties of Eu3+ and Tb3+ Complexes with a Silica Matrix by Sol-Gel Method

    Institute of Scientific and Technical Information of China (English)

    王淑萍; 王瑞芬; 张建军; 刘翠格

    2003-01-01

    Ternary complexes of europium and terbium with benzoic acid and 1, 10-phenanthroline [RE(BA)3phen] (BA=benzoate phen=1,10-phenanthroline) were introduced into a silica matrix by sol-gel method. The thermal stability and luminescence behavior of the complexes in silica gels were studied in comparison with the corresponding solid-state complexes by thermal decomposition, excitation and emission spectra. The thermal stability of the complexes is enhanced in silica gel matrix and the luminescence remaines unchanged.

  1. Gel/Space Ratio Evolution in Ternary Composite System Consisting of Portland Cement, Silica Fume, and Fly Ash

    Directory of Open Access Journals (Sweden)

    Mengxue Wu

    2017-01-01

    Full Text Available In cement-based pastes, the relationship between the complex phase assemblage and mechanical properties is usually described by the “gel/space ratio” descriptor. The gel/space ratio is defined as the volume ratio of the gel to the available space in the composite system, and it has been widely studied in the cement unary system. This work determines the gel/space ratio in the cement-silica fume-fly ash ternary system (C-SF-FA system by measuring the reaction degrees of the cement, SF, and FA. The effects that the supplementary cementitious material (SCM replacements exert on the evolution of the gel/space ratio are discussed both theoretically and practically. The relationship between the gel/space ratio and compressive strength is then explored, and the relationship disparities for different mix proportions are analyzed in detail. The results demonstrate that the SCM replacements promote the gel/space ratio evolution only when the SCM reaction degree is higher than a certain value, which is calculated and defined as the critical reaction degree (CRD. The effects of the SCM replacements can be predicted based on the CRD, and the theological predictions agree with the test results quite well. At low gel/space ratios, disparities in the relationship between the gel/space ratio and the compressive strength are caused by porosity, which has also been studied in cement unary systems. The ratio of cement-produced gel to SCM-produced gel ( G C to G S C M ratio is introduced for use in analyzing high gel/space ratios, in which it plays a major role in creating relationship disparities.

  2. Nanostructural analysis of water distribution in hydrated multicomponent gels using thermal analysis and NMR relaxometry.

    Science.gov (United States)

    Codoni, Doroty; Belton, Peter; Qi, Sheng

    2015-06-01

    Highly complex, multicomponent gels and water-containing soft materials have varied applications in biomedical, pharmaceutical, and food sciences, but the characterization of these nanostructured materials is extremely challenging. The aim of this study was to use stearoyl macrogol-32 glycerides (Gelucire 50/13) gels containing seven different species of glycerides, PEG, and PEG-esters, as model, complex, multicomponent gels, to investigate the effect of water content on the micro- and nanoarchitecture of the gel interior. Thermal analysis and NMR relaxometry were used to probe the thermal and diffusional behavior of water molecules within the gel network. For the highly concentrated gels (low water content), the water activity was significantly lowered due to entrapment in the dense gel network. For the gels with intermediate water content, multiple populations of water molecules with different thermal responses and diffusion behavior were detected, indicating the presence of water in different microenvironments. This correlated with the network architecture of the freeze-dried gels observed using SEM. For the gels with high water content, increased quantities of water with similar diffusion characteristics as free water could be detected, indicating the presence of large water pockets in these gels. The results of this study provide new insights into structure of Gelucire gels, which have not been reported before because of the complexity of the material. They also demonstrate that the combination of thermal analysis and NMR relaxometry offers insights into the structure of soft materials not available by the use of each technique alone. However, we also note that in some instances the results of these measurements are overinterpreted and we suggest limitations of the methods that must be considered when using them.

  3. Fast adsorption of p-nitrophenol from aqueous solution using β-cyclodextrin grafted silica gel

    Energy Technology Data Exchange (ETDEWEB)

    Shen, Hai-Min, E-mail: haimshen@zjut.edu.cn [College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014 (China); Zhu, Gong-Yuan; Yu, Wu-Bin; Wu, Hong-Ke [College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014 (China); Ji, Hong-Bing [School of Chemistry and Chemical Engineering, Sun Yat-sen University, Guangzhou 510275 (China); Shi, Hong-Xin; She, Yuan-Bin; Zheng, Yi-Fan [College of Chemical Engineering, Zhejiang University of Technology, Hangzhou 310014 (China)

    2015-11-30

    Graphical abstract: Fast-adsorption of pollutant p-nitrophenol from aqueous phase can be achieved through graft of reproducible β-CD onto the surface of silica gel and in the graft process only one hydroxyl of the patent β-CD was employed. The fast-adsorption performance is mainly attributed to the maintenance of the hydrophobic cavity of β-CD and no diffusion resistance existing. - Highlights: • Fast adsorption of p-nitrophenol was obtained via surface graft of β-cyclodextrin. • Maintenance of the hydrophobic cavity of β-cyclodextrin favors fast adsorption. • Adsorption equilibrium can be reached in 5 s with adsorption capacity of 41.5 mg/g. • A strategy to increase adsorption rate of adsorbent based on β-cyclodextrin obtained. • Adsorption mechanism was speculated as inclusion and hydrogen bond interaction. - Abstract: Renewable β-cyclodextrin (β-CD) was grafted onto the surface of silica gel using (3-chloropropyl)trimethoxysilane and ethylenediamine as linking groups to construct adsorbent in water treatment (CD@Si), and the obtained CD@Si was characterized through FT-IR, XPS, contact angle measurement, TGA, solid-state {sup 13}C NMR, SEM, and XRD analyses. The effects of initial pH, contact time on the adsorption performance of CD@Si to p-nitrophenol, and the adsorption kinetics, adsorption isotherms, adsorption thermodynamics, reusability and adsorption mechanism were investigated systematically, which indicate the adsorption of p-nitrophenol onto CD@Si is a very fast process and the adsorption equilibrium can be reached in 5 s with acceptable equilibrium adsorption capacity of 41.5 mg/g in pH ≥8.5, much faster than many reported adsorbents based on β-CD. The adsorption of p-nitrophenol onto CD@Si follows the pseudo-second-order model, obeys the Freundlich model, and is a feasible, spontaneous and exothermic process which is more favorable in lower temperature. And the formation of inclusion complex and hydrogen bond interaction are two

  4. Asymmetric bioreduction of acetophenones by Baker's yeast and its cell-free extract encapsulated in sol–gel silica materials

    Energy Technology Data Exchange (ETDEWEB)

    Kato, Katsuya, E-mail: katsuya-kato@aist.go.jp [National Institute of Advanced Industrial Science and Technology (AIST), 2266-98 Anagahora, Shimoshidami, Moriyama-ku, Nagoya, 463-8560 (Japan); Nakamura, Hitomi [National Institute of Advanced Industrial Science and Technology (AIST), 2266-98 Anagahora, Shimoshidami, Moriyama-ku, Nagoya, 463-8560 (Japan); Nakanishi, Kazuma [Department of Chemistry for Materials, Graduate School of Engineering, Mie University, 1577 Kurimamachiya-cho, Tsu, Mie, 514-8570 (Japan)

    2014-02-28

    Baker's yeast (BY) encapsulated in silica materials was synthesized using a yeast cell suspension and its cell-free extract during a sol–gel reaction of tetramethoxysilane with nitric acid as a catalyst. The synthesized samples were fully characterized using various methods, such as scanning electron microscopy, nitrogen adsorption–desorption, Fourier transform infrared spectroscopy, thermogravimetry, and differential thermal analysis. The BY cells were easily encapsulated inside silica-gel networks, and the ratio of the cells in the silica gel was approximately 75 wt%, which indicated that a large volume of BY was trapped with a small amount of silica. The enzyme activity (asymmetric reduction of prochiral ketones) of BY and its cell-free extract encapsulated in silica gel was investigated in detail. The activities and enantioselectivities of free and encapsulated BY were similar to those of acetophenone and its fluorine derivatives, which indicated that the conformation structure of BY enzymes inside silica-gel networks did not change. In addition, the encapsulated BY exhibited considerably better solvent (methanol) stability and recyclability compared to free BY solution. We expect that the development of BY encapsulated in sol–gel silica materials will significantly impact the industrial-scale advancement of high-efficiency and low-cost biocatalysts for the synthesis of valuable chiral alcohols.

  5. The evaluation of physical properties and in vitro cell behavior of PHB/PCL/sol-gel derived silica hybrid scaffolds and PHB/PCL/fumed silica composite scaffolds.

    Science.gov (United States)

    Ding, Yaping; Yao, Qingqing; Li, Wei; Schubert, Dirk W; Boccaccini, Aldo R; Roether, Judith A

    2015-12-01

    PHB/PCL/sol-gel derived silica hybrid scaffolds (P5S1S) and PHB/PCL/fumed silica composite scaffolds (P5S1N) with a 5:1 organic/inorganic ratio were fabricated through a combination of electrospinning and sol-gel methods and dispersion electrospinning, respectively. In contrast to the silica nanoparticle aggregates appearing on the fiber surface of P5S1N, smooth and uniform fibers were obtained for P5S1S. The fiber diameter distribution, tensile strength, thermal gravimetric analysis (TGA), and cellular behavior of both types of scaffolds were characterized and studied. The tensile strength results and TGA indicated that the interfacial interaction between the organic and the inorganic phase was enhanced in P5S1S over the nanocomposite scaffolds, and cells exhibited significantly higher alkaline phosphate activity (ALP) for P5S1S, which makes P5S1S hybrid scaffolds candidate materials for bone tissue engineering applications.

  6. Corrections for Measurements of Tritium in Subterranean Vapor using Silica Gel

    Energy Technology Data Exchange (ETDEWEB)

    Whicker, Jeffrey [Los Alamos National Laboratory; Dewart, Jean M [Los Alamos National Laboratory; Allen, Shannon P [Los Alamos National Laboratory; Eisele, William F [Los Alamos National Laboratory; Mcnaughton, Michael C [Los Alamos National Laboratory; Green, Andrew A [Los Alamos National Laboratory

    2009-01-01

    Hazardous contaminants buried within vadose zones can accumulate in soil gas. The concentrations and spatial extent of these contaminants are measured to evaluate potential transport to ground water for public risk evaluation. Tritium is an important contaminant found in and monitored for in vadose zones across numerous sites within the United States nuclear weapons complex, including Los Alamos National Laboratory. The extraction, collection, and laboratory analysis of tritium from subterranean soil gas presents numerous technical challenges that have not been fully studied. Particularly, the lack of soil moisture in the soil gas in the vadose zone makes it difficult to obtain enough sample moisture (e.g., > 5 g) to provide for the required sensitivity, and often, only small amounts of moisture can be collected. Further, although silica gel has high affinity for water vapor and is prebaked prior to sampling, there is still sufficient residual moisture in the prebaked gel to dilute the relatively small amount of sampled moisture; thereby, significantly lowering the 'true' tritium concentration in the soil gas. This paper provides an evaluation of the magnitude of the bias from dilution, provides methods to correct past measurements by applying a correction factor (CF), and evaluates the uncertainty of the CF values. For this, ten-thousand Monte Carlo calculations were perfonned and distribution parameters of CF values were detennined and evaluated. The mean and standard deviation of the distribution of CF values were 1.53 {+-} 0.36, and the minimum, median, and maximum values were 1.14, 1.43, and 5.27, respectively.

  7. Corrections for measurements of tritium in subterranean vapor using silica gel.

    Science.gov (United States)

    Whicker, Jeffrey J; Dewart, Jean M; Allen, Shannon P; Eisele, William F; McNaughton, Michael W; Green, Andrew A

    2011-01-01

    Hazardous contaminants buried within vadose zones can accumulate in soil gas. The concentrations and spatial extent of these contaminants are measured to evaluate potential transport to groundwater for public risk evaluation. Tritium is an important contaminant found and monitored for in vadose zones across numerous sites within the US nuclear weapons complex, including Los Alamos National Laboratory. The extraction, collection, and laboratory analysis of tritium from subterranean soil gas presents numerous technical challenges that have not been fully studied. Particularly, the lack of moisture in the soil gas in the vadose zone makes it difficult to obtain enough sample (e.g., > 5 g) to provide for the required measurement sensitivity, and often, only small amounts of moisture can be collected. Further, although silica gel has high affinity for water vapor and is prebaked prior to sampling, there is still sufficient residual moisture in the prebaked gel to dilute the relatively small amount of sampled moisture; thereby, significantly lowering the "true" tritium concentration in the soil gas. This paper provides an evaluation of the magnitude of the bias from dilution, provides methods to correct past measurements by applying a correction factor (CF), and evaluates the uncertainty of the CF values. For this, 10,000 Monte Carlo calculations were performed, and distribution parameters of CF values were determined and evaluated. The mean and standard deviation of the distribution of CF values were 1.53 ± 0.36, and the minimum, median, and maximum values were 1.14, 1.43, and 5.27, respectively.

  8. An improved bonded-polydimethylsiloxane solid-phase microextraction fiber obtained by a sol-gel/silica particle blend.

    Science.gov (United States)

    Azenha, Manuel; Nogueira, Pedro; Fernando-Silva, A

    2008-03-10

    A novel procedure for solid-phase microextraction fiber preparation is presented, which combines the use of a rigid titanium alloy wire as a substrate with a blend of PDMS sol-gel mixture/silica particles, as a way of increasing both the mechanical robustness and the extracting capability of the sol-gel fibers. The approximately 30 microm average thick fibers displayed an improvement in the extraction capacity as compared to the previous sol-gel PDMS fibers, due to a greater load of stable covalently bonded sol-gel PDMS. The observed extraction capacity was comparable to that of 100 microm non-bonded PDMS fiber, having in this case the advantages of the superior robustness and stability conferred, respectively, by the unbreakable substrate and the sol-gel intrinsic characteristics. Repeatability (n=3) ranged 1-8% while fiber production reproducibility (n=3) ranged 15-25%. The presence of the silica particles was found to have no direct influence on the kinetics and mechanism of the extraction process, thus being possible to consider the new procedure as a refinement of the previous ones. The applicability potential of the devised fiber was illustrated with the analysis of gasoline under the context of arson samples.

  9. Determination of arsenate in water by anion selective membrane electrode using polyurethane-silica gel fibrous anion exchanger composite.

    Science.gov (United States)

    Khan, Asif Ali; Shaheen, Shakeeba

    2014-01-15

    Polyurethane (PU)-silica (Si gel) based fibrous anion exchanger composites were prepared by solid-gel polymerization of polyurethane in the presence of different amounts of silica gel. The formation of PU-Si gel fibrous anion exchanger composite was characterized by Fourier transform infra-red spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis (TGA-DTA), scanning electron microscopy (SEM) and elemental analysis. The membrane having a composition of 5:3 (PU:Si gel) shows best results for water content, porosity, thickness and swelling. Our studies show that the present ion selective membrane electrode is selective for arsenic, having detection limit (1×10(-8)M to 1×10(-1)M), response time (45s) and working pH range (5-8). The selectivity coefficient values for interfering ions indicate good selectivity for arsenate (AsO4(3-)) over interfering anions. The accuracy of the detection limit results was compared by PCA-Arsenomat.

  10. Solid phase extraction using silica gel modified with murexide for preconcentration of uranium (VI) ions from water samples

    Energy Technology Data Exchange (ETDEWEB)

    Sadeghi, S. [Department of Chemistry, Faculty of Science, Birjand University, Birjand (Iran, Islamic Republic of)], E-mail: ssadeghi@birjand.ac.ir; Sheikhzadeh, E. [Department of Chemistry, Faculty of Science, Birjand University, Birjand (Iran, Islamic Republic of)

    2009-04-30

    Murexide was chemically bonded to silica gel surface immobilized 3-aminopropyl trimethoxysilane (APMS) to produce the new sorbent. A solid phase extraction method using the new sorbent has been developed to separate and concentrate trace amount of uranium (VI) from aqueous samples for the measurement by spectrophotometry method using Arsenazo III reagent. The influences of some analytical parameters on the quantitative recoveries of the analyte were investigated both in batch and column methods. Quantitative recovery of U(VI) was achieved by stripping with 0.1 mol L{sup -1} HCl. The maximum sorption capacity of the modified silica gel was 1.13 mmol g{sup -1} U(VI). A high preconcentration factor value of 400 with a lower limit of detection of 1 {mu}g L{sup -1} was obtained for U(VI). The practical applicability of the developed sorbent was examined using synthetic and real samples such as sea/ground water samples.

  11. 3-D mapping with ellipsometrically determined physical thickness/refractive index of spin coated sol–gel silica layer

    Indian Academy of Sciences (India)

    S Das; P Pal; S Roy; S Chakraboarty; P K Biswas

    2002-11-01

    Precursor sol for sol–gel silica layer was prepared from the starting material, tetraethylorthosilicate (TEOS). The sol was deposited onto borosilicate crown (BSC) glass by the spinning technique (rpm 2500). The gel layer thus formed transformed to oxide layer on heating to 450°C for ∼ 30 min. The physical thicknessand the refractive index of the layer were measured ellipsometrically (Rudolph Auto EL II) at 632.8 nm. About 10 × 10 mm surface area of the silica layer was chosen for evaluation of thickness and refractive index values at different points (121 nos.) with 1 mm gap between two points. Those data were utilized in the Autolisp programme for 3-D mapping. Radial distribution of the evaluated values was also displayed.

  12. Solid phase extraction using silica gel modified with murexide for preconcentration of uranium (VI) ions from water samples.

    Science.gov (United States)

    Sadeghi, S; Sheikhzadeh, E

    2009-04-30

    Murexide was chemically bonded to silica gel surface immobilized 3-aminopropyl trimethoxysilane (APMS) to produce the new sorbent. A solid phase extraction method using the new sorbent has been developed to separate and concentrate trace amount of uranium (VI) from aqueous samples for the measurement by spectrophotometry method using Arsenazo III reagent. The influences of some analytical parameters on the quantitative recoveries of the analyte were investigated both in batch and column methods. Quantitative recovery of U(VI) was achieved by stripping with 0.1 mol L(-1) HCl. The maximum sorption capacity of the modified silica gel was 1.13 mmol g(-1) U(VI). A high preconcentration factor value of 400 with a lower limit of detection of 1 microg L(-1) was obtained for U(VI). The practical applicability of the developed sorbent was examined using synthetic and real samples such as sea/ground water samples.

  13. Chemical modification of silica gel with synthesized new Schiff base derivatives and sorption studies of cobalt (II) and nickel (II)

    Energy Technology Data Exchange (ETDEWEB)

    Kursunlu, Ahmed Nuri, E-mail: ankursunlu@gmail.com [Department of Chemistry, Selcuk University, Campus, 42075, Konya (Turkey); Guler, Ersin; Dumrul, Hakan; Kocyigit, Ozcan; Gubbuk, Ilkay Hilal [Department of Chemistry, Selcuk University, Campus, 42075, Konya (Turkey)

    2009-08-15

    In this study, three Schiff base ligands and their complexes were synthesized and characterized by infrared spectroscopy (IR), thermogravimetric analyses (TGA), nuclear magnetic resonance (NMR), elemental analysis and magnetic susceptibility apparatuses. Silica gel was respectively modified with Schiff base derivatives, (E)-2-[(2-chloroethylimino)methyl]phenol, (E)-4-[(2-chloroethylimino)methyl]phenol and N,N'-[1,4-phenilendi(E)methylidene]bis(2-chloroethanamine), after silanization of silica gel by (3-aminopropyl)trimethoxysilane (APTS) by using a suitable method. Characterization of the surface modification was also performed with IR, TGA and elemental analysis. The immobilized surfaces were used for Co(II) and Ni(II) sorption from aqueous solutions and values of sorption were detected by atomic absorption spectrometer (AAS).

  14. Sugarcane bagasse lignin, and silica gel and magneto-silica as drug vehicles for development of innocuous methotrexate drug against rheumatoid arthritis disease in albino rats

    Energy Technology Data Exchange (ETDEWEB)

    Wahba, Sanaa M.R. [Zoology department, Women College, Ain-Shams University,11566 Cairo (Egypt); Darwish, Atef S., E-mail: atef_mouharam@sci.asu.edu.eg [Chemistry department, Faculty of Science, Ain Shams University, Cairo (Egypt); Shehata, Iman H. [Microbiology and Immunology Department, Faculty of Medicine, Ain-Shams University, Cairo (Egypt); Abd Elhalem, Sahar S. [Zoology department, Women College, Ain-Shams University,11566 Cairo (Egypt)

    2015-03-01

    The present study clarifies co-therapy action of deliveries from their textural changes point of view. Methotrexate (MTX) was immobilized onto biodegradable lignin, silica gel and iron/silica nanocomposite. Loaded-MTX was i.p. injected into albino rats at doses of 0.25 and 0.5 mg/kg/week for 2.5 months, after which spleen, liver, testes and knee joint tissues were collected for tests. IFN-γ and IL-17A mRNA gene expressions in spleen in all biological samples were determined by RT-PCR. Physicochemical features of drug carriers were monitored by XRD, BET-PSD, SEM and TEM. Drug inflammatory-site targeting was found to be closely related to the physico-features of deliverers. The interlayered lignin of micro- and meso-pore channels directed MTX toward concealed infected cells in liver and testes tissues, while meso-structured silica flacks satisfied by gathering MTX around knee joints. The magneto-silica nanocomposite targeted MTX toward spleen tissue, which is considered as a lively factory for the production of electron rich compounds. - Highlights: • Opening the door to synthesize smart targeted drug deliveries against RA disease • Therapy action of MTX-laden lignin and Fe{sub 3}O{sub 4}/SiO{sub 2} composite toward RA disease • Procure selective targeted drug deliveries of near 100% curing against RA disease • Revolutionary clinical therapies for RA disease by inventive MTX-delivery models.

  15. Probing the microenvironment of an oligo-(p-phenylene vinylene) derivative encapsulated in polymer-impregnated sol-gel silica matrix

    Institute of Scientific and Technical Information of China (English)

    TANG Jun; DU Chuang; YU Xiaoqiang; ZHANG Guo; WANG Ce

    2004-01-01

    Polymer-impregnated silica sol-gel composite materials are hosts for organics in advanced optics application. An oligo-phenylene vinylene derivative 4,4'-(1,4-phenylene dithenylene)-bis-(N-methyl pyridinium iodide)(OPVD) was introduced to poly(hydroxyethyl methacrylate)(PHEMA)-impregnated silica composite film by the sol-gel process. By comparing the X-ray diffraction, UV-visible spectra, steady-state and time-resolved fluorescence spectra of OPVD in three solid matrices (PHEMA/silica composite film, pure PHEMA film, and pure silica film), the similar results of PHEMA/silica composite film and pure PHEMA film demonstrate that the OPVD is primarily surrounded by a PHEMA-like environment in the composite matrix. The model of such structure is presented, which is useful for further understanding and optimizing of properties of doped sol-gel materials.

  16. Silica-gel Supported V Complexes:Preparation, Characterization and Catalytic Oxidative Desulfurization

    Institute of Scientific and Technical Information of China (English)

    黎俊波; 刘习文; 曹灿灿; 郭嘉; 潘志权

    2013-01-01

    In this manuscript, a series of catalyst SGn-[VVO2-PAMAM-MSA] (SG=silica gel, PAMAM=poly-amidoamine, MSA=5-methyl salicylaldehyde, n=0, 1, 2, 3) was prepared and their structures were fully charac-terized by Fourier transform-infrared spectroscopy (FT-IR), thermogravimetric analysis (TGA), X-ray photoelec-tron spectroscopy (XPS) and inductive coupled plasma emission spectrometer (ICP) etc. XPS revealed that the metal V and SGn-PAMAM-MSA combined more closely after the formation of Schiff base derivatives. Their cata-lytic activities for oxidation of dibenzothiophene were evaluated using tert-butyl hydroperoxide as oxidant. The results showed that the catalyst SG2.0-[VVO2-PAMAM-MSA] presented good catalytic activity and recycling time. Mean-while, the optimal condition for the catalytic oxidation of SG2.0-[VVO2-PAMAM-MSA] was also investigated, which showed that when the oxidation temperature was 90 °C, time was 60 min, the O/S was 3︰1, and the mass content of catalyst was 1%, the rate of desulfurization could reach 85.2%. Moreover, the catalyst can be recycled several times without significant decline in catalytic activity.

  17. Fast adsorption of p-nitrophenol from aqueous solution using β-cyclodextrin grafted silica gel

    Science.gov (United States)

    Shen, Hai-Min; Zhu, Gong-Yuan; Yu, Wu-Bin; Wu, Hong-Ke; Ji, Hong-Bing; Shi, Hong-Xin; She, Yuan-Bin; Zheng, Yi-Fan

    2015-11-01

    Renewable β-cyclodextrin (β-CD) was grafted onto the surface of silica gel using (3-chloropropyl)trimethoxysilane and ethylenediamine as linking groups to construct adsorbent in water treatment (CD@Si), and the obtained CD@Si was characterized through FT-IR, XPS, contact angle measurement, TGA, solid-state 13C NMR, SEM, and XRD analyses. The effects of initial pH, contact time on the adsorption performance of CD@Si to p-nitrophenol, and the adsorption kinetics, adsorption isotherms, adsorption thermodynamics, reusability and adsorption mechanism were investigated systematically, which indicate the adsorption of p-nitrophenol onto CD@Si is a very fast process and the adsorption equilibrium can be reached in 5 s with acceptable equilibrium adsorption capacity of 41.5 mg/g in pH ≥8.5, much faster than many reported adsorbents based on β-CD. The adsorption of p-nitrophenol onto CD@Si follows the pseudo-second-order model, obeys the Freundlich model, and is a feasible, spontaneous and exothermic process which is more favorable in lower temperature. And the formation of inclusion complex and hydrogen bond interaction are two origins of p-nitrophenol being adsorbed onto CD@Si. Additionally, CD@Si can be recycled and reused at least five runs with acceptable adsorption capacity, is a very promising adsorbent in the fast adsorption of p-nitrophenol or its analogues from aqueous phase.

  18. Adsorption of Pb(II) from aqueous solution by silica-gel supported hyperbranched polyamidoamine dendrimers.

    Science.gov (United States)

    Niu, Yuzhong; Qu, Rongjun; Sun, Changmei; Wang, Chunhua; Chen, Hou; Ji, Chunnuan; Zhang, Ying; Shao, Xia; Bu, Fanling

    2013-01-15

    The adsorption properties of silica-gel supported hyperbranched polyamidoamine dendrimers (SiO(2)-G0-SiO(2)-G4.0) have been investigated by batch method. The effect of pH of the solution, contact time, initial Pb(II) ion concentration, temperature and coexisting metal ions have been demonstrated. The results indicated that the optimum pH value was 5. Adsorption kinetics was found to follow the pseudo-second-order model and controlled by film diffusion. The adsorption isotherms were fitted by Langmuir, Freundlich and Dubinin-Radushkevich (D-R) isotherm models. Langmuir isotherm model was found to be more suitable to describe the equilibrium data, suggesting the uptake of Pb(II) ions by monolayer adsorption. From D-R isotherm model, the calculated mean free energy E demonstrated the adsorption processes occurred by chemical ion-exchange mechanism. FTIR analysis revealed that amine groups were mainly responsible for the adsorption of Pb(II) by amino-terminated adsorbents, while CO of ester groups also participated in the adsorption process of ester-terminated ones. The adsorbents can selectively adsorb Pb(II) from binary ion systems in the presence of Mn(II), Cu(II), Co(II), and Ni(II). Based on the results, it is concluded that SiO(2)-G0-SiO(2)-G4.0 had great potential for the removal of Pb(II) from aqueous solution.

  19. Synthesis of Au-Ag alloy nanoparticles supported on silica gel via galvanic replacement reaction

    Institute of Scientific and Technical Information of China (English)

    Xiaoyan Liu; Aiqin Wang; Lin Li; Tao Zhang; Chung-Yuan Mou; Jyh-Fu Lee

    2013-01-01

    Synthesis of supported Au-Ag bimetallic has attracted much attention since we found for the first time that Au and Ag had synergistic effect on CO oxidation and preferential CO oxidation in rich hydrogen. In this work, the formation of Au-Ag alloy nanoparticles supported on silica gel by galvanic replacement reaction has been investigated. We applied various characterizations including X-ray diffraction (XRD), transmission electronic microscopy (TEM), ultraviolet-visible spectroscopy (UV-vis), X-ray absorption spectroscopy (XAS) to characterize the formation process of Au-Ag alloy. Although the average particle sizes of the Au-Ag alloy nanoparticles obtained by the galvanic replacement reaction are relatively large comparing with that of loading Au first, the catalytic activity of the catalyst in preferential CO oxidation is almost the same. This result manifested that the particle size effect of Au-Ag nanoparticles was not as tremendous as that of monometallic gold. The formation of Au-Ag alloy made it less sensitive to the particle size.

  20. Static Analysis of Double Effect Adsorption Refrigeration Cycle Using Silica gel/Water Pair

    Science.gov (United States)

    Marlinda; Miyazaki, Takahiko; Ueda, Yuki; Akisawa, Atsushi

    In this paper,a static analysis of double effect adsorption refrigeration cycle utilizing condensation heat is discussed. Double effect adsorption refrigeration cycle consists of two cycles, High Temperature Cycle (HTC) which is driven from external heat sources, and Low Temperature Cycle (LTC) which is driven by condensation heat from HTC. Both of HTC and LTC are using silica gel and water as working pairs. The effect of heat source temperature on cycle performance was investigated in terms of coefficient of performance (COP) and specific cooling energy (SCE). Results showed that double effect cycle would produce higher COP than single effect cycle for driving temperature observed between 80-150°C with the same operating condition. However, the value of SCE is lower than single effect, despite that the SCE of double effect cycle is improved with heat source temperature higher than 100°C. Further, it was also observed that adsorbent mass ratio of HTC and LTC affected performance of chiller. When adsorbent mass ratio of HTC and LTC was unity, it was found that SCE and COP took the maximum.

  1. Computational Analysis of Silica gel-Water Adsorption Refrigeration Cycle with Mass Recovery

    Science.gov (United States)

    Akahira, Akira; Alam, K. C. Amanul; Hamamoto, Yoshinori; Akisawa, Atsushi; Kashiwagi, Takao

    The study aims at clarifying the performance of silica gel-water adsorption refrigeration cycle with mass recovery process.Two kinds of heat exchanger were examined and the performances were compared with each other. One type of heat exchanger was a spiral tube and it was immersed in a low temperature thermostatic bath. The other was coil-shaped double tube heat exchanger using two tubes. The emulsion was circulated to make ice continuously. These systems were operated under various cooling conditions (flow rates of the emulsion and brine temperatures). The effects of the tube materials (fluororesin and non-fluororesin) and thickness were also examined. Slurry ice was formed continuously without adhesion of ice to the cooling wall under certain conditions. Using the fluororesin tube prevented ice from the adhesion and it enlarged the range of the cooling conditions under which slurry ice was formed continuously. Furthermore, by making thickness of the tube thinner and increasing the heat transfer coefficient on the outside of the tube, ice was made continuously without lowering the rate of ice formation at a higher brine temperature.

  2. Study of a novel silica gel-water adsorption chiller. Part II. Experimental study

    Energy Technology Data Exchange (ETDEWEB)

    Wang, D.C.; Wu, J.Y.; Xia, Z.Z.; Zhai, H.; Wang, R.Z. [Institute of Refrigeration and Cryogenics, Shanghai Jiaotong University, Shanghai 200030 (China); Dou, W.D. [Jiangsu Shuangliang Air Conditioning Equipment Co., Ltd, Jiangsu 214444 (China)

    2005-11-01

    The prototype of a novel silica gel-water adsorption chiller is built and its performance is tested in detail. The experimental results show that the refrigerating capacity (RC) and COP of the chiller are 7.15 and 0.38kW, respectively, when the hot water temperature is 84.8{sup o}C, the cooling water temperature is 30.6{sup o}C, and the chilled water outlet temperature is 11.7{sup o}C. The RC will reach 6kW under the condition of 65{sup o}C hot water temperature, 30.5{sup o}C cooling water temperature and 17.6{sup o}C chilled water temperature. The results confirm that this kind of adsorption chiller is an effective refrigerating machine though its performance is not as fine as the prediction results. Also it is well effectively driven by a low-grade heat source. Therefore, its applications to the low-grade heat source are much attractive. (author)

  3. Efficient and solvent-free synthesis of bis-indolylmethanes using silica gel supported aluminium chloride as a reusable catalyst

    Institute of Scientific and Technical Information of China (English)

    Kaveh Parvanak Boroujeni; Kamran Parvanak

    2011-01-01

    Stable and non-hygroscopic silica gel supported aluminium chloride (SiO2-AlCl3), which is prepared easily from cheap and commercially available compounds was found to be an environmentally friendly heterogeneous catalyst for the condensation of indole with aldehydes and ketones to afford bis-indolylmethanes at room temperature under solvent-free conditions. The catalyst can be reused up to five times after simple washing with ether.

  4. Ag nanoparticle/melamine sulfonic acid supported on silica gel as an efficient catalytic system for synthesis of dihydropyrimidinthiones

    Directory of Open Access Journals (Sweden)

    Parya Nasehi

    2014-07-01

    Full Text Available 3,4-Dihydropyrimidin-2(1H-thiones were synthesized in the presence of Ag nanoparticle/melamine sulfonic acid (MSA supported on silica gel. The reactionwas carried out at 110 oC for 20 min under solvent free conditions. This method hassome advantages such as good yield, mild reaction conditions, ease of operation and work up, short reaction time and high product purity.

  5. Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films

    Energy Technology Data Exchange (ETDEWEB)

    Saison, Tamar; Peroz, Christophe; Chauveau, Vanessa; Sondergard, Elin; Arribart, Herve [Unite mixte CNRS/Saint Gobain Saint Gobain Recherche, BP135, 93303 Aubervilliers (France); Berthier, Serge [Institut des Nanosciences de Paris, UMR 7588, CNRS, Universite Pierre et Marie Curie-Paris 6, 140 rue Lourmel, 75015 Paris (France)], E-mail: cperoz@lbl.gov

    2008-12-01

    An original and low cost method for the fabrication of patterned surfaces bioinspired from butterfly wings and lotus leaves is presented. Silica-based sol-gel films are thermally imprinted from elastomeric molds to produce stable structures with superhydrophobicity values as high as 160 deg. water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 deg. C and 500 deg. C.

  6. Replication of butterfly wing and natural lotus leaf structures by nanoimprint on silica sol-gel films.

    Science.gov (United States)

    Saison, Tamar; Peroz, Christophe; Chauveau, Vanessa; Berthier, Serge; Sondergard, Elin; Arribart, Hervé

    2008-12-01

    An original and low cost method for the fabrication of patterned surfaces bioinspired from butterfly wings and lotus leaves is presented. Silica-based sol-gel films are thermally imprinted from elastomeric molds to produce stable structures with superhydrophobicity values as high as 160 degrees water contact angle. The biomimetic surfaces are demonstrated to be tuned from superhydrophobic to superhydrophilic by annealing between 200 degrees C and 500 degrees C.

  7. Effect of silver ions on the energy transfer from host defects to Tb ions in sol–gel silica glass

    Energy Technology Data Exchange (ETDEWEB)

    Abbass, Abd Ellateef [Department of Physics, University of the Free State, Bloemfontein (South Africa); Department of Physics, Sudan University of Science and Technology (Sudan); Swart, H.C. [Department of Physics, University of the Free State, Bloemfontein (South Africa); Kroon, R.E., E-mail: KroonRE@ufs.ac.za [Department of Physics, University of the Free State, Bloemfontein (South Africa)

    2015-04-15

    Plasmonic metal structures have been suggested to enhance the luminescence from rare-earth (RE) ions, but this enhancement is not yet well understood or applied to phosphor materials. Although some reports using Ag nanoparticles (NPs) in glass have attributed enhancement of RE emission to the strong electric fields associated with Ag NPs, it has also been proposed that the enhancement is instead due to energy transfer from Ag ions to RE ions. Our work using sol–gel silica shows a third possibility, namely that enhancement of the RE (e.g. Tb) emission is due to energy transfer from defects of the host material to the Tb ions, where the addition of Ag influences the silica host defects. The oxidation state of Ag as a function of annealing temperature was investigated by x-ray diffraction, transmission electron microscopy, UV–vis measurements and x-ray photoelectron spectroscopy, while optical properties were investigated using a Cary Eclipse fluorescence spectrophotometer or by exciting samples with a 325 nm He–Cd laser. The results showed that Ag ions have a significant effect on the silica host defects, which resulted in enhancement of the green Tb emission at 544 nm for non-resonant excitation using a wavelength of 325 nm. - Highlights: • Conversion of Ag ions to metallic nanoparticles after annealing of sol–gel silica. • Addition of Ag resulted in enhanced green luminescence from Tb ions in silica. • Enhancement is attributed to the effect of added Ag on the host defects of silica.

  8. Surface Behavior of Rhodamin and Tartrazine on Silica-Cellulose Sol-Gel Surfaces by Thin Layer Elution

    Directory of Open Access Journals (Sweden)

    Surjani Wonorahardjo

    2016-05-01

    Full Text Available Physical and chemical interactions are the principles for different types of separation systems as the equillibrium dynamics on surface plays a key-role. Surface modification is a way for selective separation at interfaces. Moreover, synthesis of gel silica by a sol-gel method is preferred due to the homogeneity and surface feature easily controlled. Cellulose can be added in situ to modified the silica features during the process. Further application for to study interaction of rhodamin and tartrazine in its surface and their solubilities in mobile phase explains the possibility for their separation. This paper devoted to evaluate the surface behavior in term of adsorption and desorption of tartrazine and rhodamin on silica-cellulose thin layer in different mobile phase. Some carrier liquids applied such as methanol, acetone, n-hexane and chloroform. The result proves tartrazine and rhodamin is separated and have different behavior in different mobile phase. The retardation factors (Rf of the mixtures suggest complexity behavior on silica-cellulose surface.

  9. Synthesis and characterization of cellulose-functionalized 3,4-dihydroxyphenylalanine(dopamine)/silica-gold nanomaterials by sol-gel process.

    Science.gov (United States)

    Ramesh, Sivalingam; Kim, Joo-Hyung

    2012-10-01

    Cellulose-metal oxide nanomaterials were developed the technologies to manipulate self-assembly and multi-functionallity, of new technologies to the point where industry can produce advanced and cost-competitive cellulose and lignocellulose-based materials. The present investigation focused on cellulose-silica and cellulose functionalized 3,4-dihydroxy phenyl alanine(dopamine) silica/gold nanomaterials by in-situ sol-gel process. The tetraethoxysilane (TEOS) and gold precursors such as tetrachloroauricacid (HAuCl4) and γ- aminopropyltriethoxysilane (γ-APTES) as coupling agent were used for sol-gel crosslinking process. The chemical and morphological properties of cellulose/silica and cellulose /silica-gold nanomaterials via covalent crosslinking hybrids were investigated with FTIR, XRD, SEM and TEM analysis. The results show that cellulose/silica and cellulose functionalized dopamine-silica/gold hybrids form new macromolecular structures in the size of 20 nm.

  10. Integrating nanohybrid membranes of reduced graphene oxide: chitosan: silica sol gel with fiber optic SPR for caffeine detection.

    Science.gov (United States)

    Kant, Ravi; Tabassum, Rana; Gupta, Banshi D

    2017-05-12

    Caffeine is the most popular psychoactive drug consumed in the world for improving alertness and enhancing wakefulness. However, caffeine consumption beyond limits can result in lot of physiological complications in human beings. In this work, we report a novel detection scheme for caffeine integrating nanohybrid membranes of reduced graphene oxide (rGO) in chitosan modified silica sol gel (rGO: chitosan: silica sol gel) with fiber optic surface plasmon resonance. The chemically synthesized nanohybrid membrane forming the sensing route has been dip coated over silver coated unclad central portion of an optical fiber. The sensor works on the mechanism of modification of dielectric function of sensing layer on exposure to analyte solution which is manifested in terms of red shift in resonance wavelength. The concentration of rGO in polymer network of chitosan and silica sol gel and dipping time of the silver coated probe in the solution of nanohybrid membrane have been optimized to extricate the supreme performance of the sensor. The optimized sensing probe possesses a reasonably good sensitivity and follows an exponentially declining trend within the entire investigating range of caffeine concentration. The sensor boasts of an unparalleled limit of detection value of 1.994 nM and works well in concentration range of 0-500 nM with a response time of 16 s. The impeccable sensor methodology adopted in this work combining fiber optic SPR with nanotechnology furnishes a novel perspective for caffeine determination in commercial foodstuffs and biological fluids.

  11. Integrating nanohybrid membranes of reduced graphene oxide: chitosan: silica sol gel with fiber optic SPR for caffeine detection

    Science.gov (United States)

    Kant, Ravi; Tabassum, Rana; Gupta, Banshi D.

    2017-05-01

    Caffeine is the most popular psychoactive drug consumed in the world for improving alertness and enhancing wakefulness. However, caffeine consumption beyond limits can result in lot of physiological complications in human beings. In this work, we report a novel detection scheme for caffeine integrating nanohybrid membranes of reduced graphene oxide (rGO) in chitosan modified silica sol gel (rGO: chitosan: silica sol gel) with fiber optic surface plasmon resonance. The chemically synthesized nanohybrid membrane forming the sensing route has been dip coated over silver coated unclad central portion of an optical fiber. The sensor works on the mechanism of modification of dielectric function of sensing layer on exposure to analyte solution which is manifested in terms of red shift in resonance wavelength. The concentration of rGO in polymer network of chitosan and silica sol gel and dipping time of the silver coated probe in the solution of nanohybrid membrane have been optimized to extricate the supreme performance of the sensor. The optimized sensing probe possesses a reasonably good sensitivity and follows an exponentially declining trend within the entire investigating range of caffeine concentration. The sensor boasts of an unparalleled limit of detection value of 1.994 nM and works well in concentration range of 0-500 nM with a response time of 16 s. The impeccable sensor methodology adopted in this work combining fiber optic SPR with nanotechnology furnishes a novel perspective for caffeine determination in commercial foodstuffs and biological fluids.

  12. Transition metal-free oxidation of benzylic alcohols to carbonyl compounds by hydrogen peroxide in the presence of acidic silica gel

    Directory of Open Access Journals (Sweden)

    Hossein Ghafuri

    2015-01-01

    Full Text Available Oxidation of alcohols to carbonyl compounds has become an important issue in the process industry as well as many other applications. In this method, various benzylic alcohols were successfully converted to corresponding aldehydes and ketones under transition metal-free condition using hydrogen peroxide in the presence of some amount of catalytic acidic silica gel. Silica gel is inexpensive and available. One of the most important features of this method is its short reaction time.

  13. Preconcentration and Determination of Mefenamic Acid in Pharmaceutical and Biological Fluid Samples by Polymer-grafted Silica Gel Solid-phase Extraction Following High Performance Liquid Chromatography

    OpenAIRE

    Bagheri Sadeghi, Hayedeh; Panahi, Homayon Ahmad; Mahabadi, Mahsa; Moniri, Elham

    2015-01-01

    Mefenamic acid is a nonsteroidal anti-inflammatory drug (NSAID) that has analgesic, anti-infammatory and antipyretic actions. It is used to relieve mild to moderate pains. Solid-phase extraction of mefenamic acid by a polymer grafted to silica gel is reported. Poly allyl glycidyl ether/iminodiacetic acid-co-N, N-dimethylacrylamide was synthesized and grafted to silica gel and was used as an adsorbent for extraction of trace mefenamic acid in pharmaceutical and biological samples. Different fa...

  14. Large Mesopore Generation in an Amorphous Silica-Alumina by Controlling the Pore Size with the Gel Skeletal Reinforcement and Its Application to Catalytic Cracking

    Directory of Open Access Journals (Sweden)

    Hiroyuki Nasu

    2012-09-01

    Full Text Available Tetraethoxy orthosilicate (TEOS was used not only as a precursor of silica, but also as an agent which reinforces the skeleton of silica-gel to prepare an aerogel and resultant silica and silica-alumina with large pore size and pore volume. In this gel skeletal reinforcement, the strength of silica aerogel skeleton was enhanced by aging with TEOS/2-propanol mixed solution to prevent the shrink of the pores. When silica aerogel was reinforced by TEOS solution, the pore diameter and pore volume of calcined silica could be controlled by the amount of TEOS solution and reached 30 nm and 3.1 cm3/g. The results from N2 adsorption measurement indicated that most of pores for this silica consisted of mesopores. Silica-alumina was prepared by the impregnation of an aluminum tri-sec-butoxide/2-butanol solution with obtained silica. Mixed catalysts were prepared by the combination of β-zeolite (26 wt% and prepared silica-aluminas with large mesopore (58 wt% and subsequently the effects of their pore sizes on the catalytic activity and the product selectivity were investigated in catalytic cracking of n-dodecane at 500 °C. The mixed catalysts exhibited not only comparable activity to that for single zeolite, but also unique selectivity where larger amounts of branched products were formed.

  15. Preparation and luminescence properties of europium complex with a-naphthylacetic acid incorporated in silica matrix by sol-gel method

    Institute of Scientific and Technical Information of China (English)

    陈野; 蔡伟民; 孙晓君; 崔丹; 于英宁

    2004-01-01

    Europium ternary complex of Eu (NNA)3(NNA=o-naphthylacetic acid) was embedded in silica matrix at different ratios by sol-gel method. The luminescence properties of silica composites were studied by comparing them with those of corresponding pure complex by means of excitation, emission spectra and lifetimes. The fluorescence lifetime was prolonged when the pure complex was incorporated in silica matrix. The relative fluorescence intensity and fluorescence lifetimes increased simultaneously with the increase of Eu(NNA)3.

  16. Determination of fluorine content in the hydrated silica%白炭黑中氟含量的测定方法

    Institute of Scientific and Technical Information of China (English)

    刘颖; 张筑南; 唐波

    2012-01-01

    介绍了利用磷肥企业含氟硅渣生产白炭黑工艺中,白炭黑中氟含量的分析方法。对氧硅酸钾法、电极法、比色法3种氟含量分析方法进行了比较,得出电极法操作简单,能快捷地分析出氟含量,是较合适的分析方法;如氟含量较高,采用氟硅酸法分析比较合适。%The article briefly had introduced the fluorine content analysis method in the hydrated silica, which was produced by fluorine silicon slag from the phosphate fertilizer enterprise. The fluorine content analysis methods including the potassium fluosilieate method,the electrode method and the colorimetric method were compared. It was drawn that the electrode method was a simple,quick analysis method of the fluorine content. So,it was more appro- priate analysis method of the fluorine content in the hydrated silica. If the hydrated silica had higher fluorine con- tent, the potassium fluosilicate analysis method was more appropriate.

  17. Preconcentration and Determination of Mefenamic Acid in Pharmaceutical and Biological Fluid Samples by Polymer-grafted Silica Gel Solid-phase Extraction Following High Performance Liquid Chromatography

    Science.gov (United States)

    Bagheri Sadeghi, Hayedeh; Panahi, Homayon Ahmad; Mahabadi, Mahsa; Moniri, Elham

    2015-01-01

    Mefenamic acid is a nonsteroidal anti-inflammatory drug (NSAID) that has analgesic, anti-infammatory and antipyretic actions. It is used to relieve mild to moderate pains. Solid-phase extraction of mefenamic acid by a polymer grafted to silica gel is reported. Poly allyl glycidyl ether/iminodiacetic acid-co-N, N-dimethylacrylamide was synthesized and grafted to silica gel and was used as an adsorbent for extraction of trace mefenamic acid in pharmaceutical and biological samples. Different factors affecting the extraction method were investigated and optimum conditions were obtained. The optimum pH value for sorption of mefenamic acid was 4.0. The sorption capacity of grafted adsorbent was 7.0 mg/g. The best eluent solvent was found to be trifluoroacetic acid-acetic acid in methanol with a recovery of 99.6%. The equilibrium adsorption data of mefenamic acid by grafted silica gel was analyzed by Langmuir model. The conformation of obtained data to Langmuir isotherm model reveals the homogeneous binding sites of grafted silica gel surface. Kinetic study of the mefenamic acid sorption by grafted silica gel indicates the good accessibility of the active sites in the grafted polymer. The sorption rate of the investigated mefenamic acid on the grafted silica gel was less than 5 min. This novel synthesized adsorbent can be successfully applied for the extraction of trace mefenamic acid in human plasma, urine and pharmaceutical samples. PMID:26330865

  18. Simultaneous removal of colour, phosphorus and disinfection from treated wastewater using an agent synthesized from amorphous silica and hydrated lime.

    Science.gov (United States)

    Yamashita, Takahiro; Aketo, Tsuyoshi; Minowa, Nobutaka; Sugimoto, Kiyomi; Yokoyama, Hiroshi; Ogino, Akifumi; Tanaka, Yasuo

    2013-01-01

    An agent synthesized from amorphous silica and hydrated lime (CSH-lime) was investigated for its ability to simultaneously remove the colour, phosphorus and disinfection from the effluents from wastewater treatment plants on swine farms. CSH-lime removed the colour and phosphate from the effluents, with the colour-removal effects especially high at pH 12, and phosphorous removal was more effective in strongly alkaline conditions (pH > 10). Colour decreased from 432 +/-111 (mean +/- SD) to 107 +/- 41 colour units and PO4(3-)P was reduced from 45 +/- 39 mg/L to undetectable levels at the CSH-lime dose of 2.0% w/v. Moreover, CSH-lime reduced the total organic carbon from 99.0 to 37.9 mg/L at the dose of 2.0% w/v and was effective at inactivating total heterotrophic and coliform bacteria. However, CSH-lime did not remove nitrogen compounds such as nitrite, nitrate and ammonium. Colour was also removed from dye solutions by CSH-lime, at the same dose.

  19. Open-Source-Based 3D Printing of Thin Silica Gel Layers in Planar Chromatography.

    Science.gov (United States)

    Fichou, Dimitri; Morlock, Gertrud E

    2017-02-07

    On the basis of open-source packages, 3D printing of thin silica gel layers is demonstrated as proof-of-principle for use in planar chromatography. A slurry doser was designed to replace the plastic extruder of an open-source Prusa i3 printer. The optimal parameters for 3D printing of layers were studied, and the planar chromatographic separations on these printed layers were successfully demonstrated with a mixture of dyes. The layer printing process was fast. For printing a 0.2 mm layer on a 10 cm × 10 cm format, it took less than 5 min. It was affordable, i.e., the running costs for producing such a plate were less than 0.25 Euro and the investment costs for the modified hardware were 630 Euro. This approach demonstrated not only the potential of the 3D printing environment in planar chromatography but also opened new avenues and new perspectives for tailor-made plates, not only with regard to layer materials and their combinations (gradient plates) but also with regard to different layer shapes and patterns. As such an example, separations on a printed plane layer were compared with those obtained from a printed channeled layer. For the latter, 40 channels were printed in parallel on a 10 cm × 10 cm format for the separation of 40 samples. For producing such a channeled plate, the running costs were below 0.04 Euro and the printing process took only 2 min. All modifications of the device and software were released open-source to encourage reuse and improvements and to stimulate the users to contribute to this technology. By this proof-of-principle, another asset was demonstrated to be integrated into the Office Chromatography concept, in which all relevant steps for online miniaturized planar chromatography are performed by a single device.

  20. Superhydrophobic films on glass surface derived from trimethylsilanized silica gel nanoparticles.

    Science.gov (United States)

    Goswami, Debmita; Medda, Samar Kumar; De, Goutam

    2011-09-01

    The paper deals with the fabrication of sol-gel-derived superhydrophobic films on glass based on the macroscopic silica network with surface modification. The fabricated transparent films were composed of a hybrid -Si(CH(3))(3)-functionalized SiO(2) nanospheres exhibiting the desired micro/nanostructure, water repellency, and antireflection (AR) property. The wavelength selective AR property can be tuned by controlling the physical thickness of the films. Small-angle X-ray scattering (SAXS) studies revealed the existence of SiO(2) nanoparticles of average size ∼9.4 nm in the sols. TEM studies showed presence of interconnected SiO(2) NPs of ∼10 nm in size. The films were formed with uniformly packed SiO(2) aggregates as observed by FESEM of film surface. FTIR of the films confirmed presence of glasslike Si-O-Si bonding and methyl functionalization. The hydrophobicity of the surface was depended on the thickness of the deposited films. A critical film thickness (>115 nm) was necessary to obtain the air push effect for superhydrophobicity. Trimethylsilyl functionalization of SiO(2) and the surface roughness (rms ≈30 nm as observed by AFM) of the films were also contributed toward the high water contact angle (WCA). The coated glass surface showed WCA value of the droplet as high as 168 ± 3° with 6 μL of water. These superhydrophobic films were found to be stable up to about 230-240 °C as confirmed by TG/DTA studies, and WCA measurements of the films with respect to the heat-treatment temperatures. These high water repellant films can be deposited on relatively large glass surfaces to remove water droplets immediately without any mechanical assistance.

  1. Effects of temperature and sodium carboxylate additives on mineralization of calcium oxalate in silica gel systems

    Institute of Scientific and Technical Information of China (English)

    OUYANG Jianming; DENG Suiping; LI Xiangping; TAN Yanhua; Bernd Tieke

    2004-01-01

    The effects of temperature and multifunctional sodium carboxylate additives on the phase composition and morphology of calcium oxalate (CaOxa) crystals grown in silica gel system were systematically investigated using scanning electron microscopy (SEM), powder X-ray diffraction (XRD), and Fourier-transform infrared spectra (FT-IR). The sodium carboxylates investigated include: monocarboxylate sodium acetate (NaAc), disodium tartrate (Na2tart), trisodium citrate (Na3cit), and the disodium salt of ethylenediaminetetraacetic acid (Na2edta). The temperature range was from 7℃ to 67℃. The crystallization temperature affects the phase compositions, the growth rate, and the morphology of CaOxa. First, the logarithm of the percentage of calcium oxalate dihydrate (COD) formed at a certain temperature (T) is proportional to the reciprocal of temperature (1/T). Second, the weight of CaOxa crystals decreases as decreasing the temperature. At a given temperature, the ability of the sodium carboxylates to induce COD follows the order: Na2edta > Na3cit > Na2tart >> NaAc. Third, the multicarboxylates can decrease the surface area of calcium oxalate monohydrate (COM).It makes the edges and tips of COM crystals blunt and oval. All the three changes, an increase of the content of COD, a decrease of the weight of CaOxa crystals, and a decrease of the surfacearea of COM crystals,can inhibit the formation of CaOxa stones. These results support the clinical use of citrates and may be helpful in elucidating the mechanisms of the formation of CaOxa calculus.

  2. Silica/quercetin sol-gel hybrids as antioxidant dental implant materials

    Science.gov (United States)

    Catauro, Michelina; Papale, Ferdinando; Bollino, Flavia; Piccolella, Simona; Marciano, Sabina; Nocera, Paola; Pacifico, Severina

    2015-06-01

    The development of biomaterials with intrinsic antioxidant properties could represent a valuable strategy for preventing the onset of peri-implant diseases. In this context, quercetin, a naturally occurring flavonoid, has been entrapped at different weight percentages in a silica-based inorganic material by a sol-gel route. The establishment of hydrogen bond interactions between the flavonol and the solid matrix was ascertained by Fourier transform infrared spectroscopy. This technique also evidenced changes in the stretching frequencies of the quercetin dienonic moiety, suggesting that the formation of a secondary product occurs. Scanning electron microscopy was applied to detect the morphology of the synthesized materials. Their bioactivity was shown by the formation of a hydroxyapatite layer on sample surface soaked in a fluid that simulates the composition of human blood plasma. When the potential release of flavonol was determined by liquid chromatography coupled with ultraviolet and electrospray ionization tandem mass spectrometry techniques, the eluates displayed a retention time that was 0.5 min less than quercetin. Collision-activated dissociation mass spectrometry and untraviolet-visible spectroscopy were in accordance with the release of a quercetin derivative. The antiradical properties of the investigated systems were evaluated by DPPH and ABTS methods, whereas the 2,7-dichlorofluorescein diacetate assay highlighted their ability to inhibit the H2O2-induced intracellular production of reactive oxygen species in NIH-3T3 mouse fibroblast cells. Data obtained, along with data gathered from the MTT cytotoxicity test, revealed that the materials that entrapped the highest amount of quercetin showed notable antioxidant effectiveness.

  3. Clathrate formation and dissociation in vapor/water/ice/hydrate systems in SBA-15, sol-gel and CPG porous media, as probed by NMR relaxation, novel protocol NMR cryoporometry, neutron scattering and ab initio quantum-mechanical molecular dynamics simulation.

    Science.gov (United States)

    Webber, J Beau W; Anderson, Ross; Strange, John H; Tohidi, Bahman

    2007-05-01

    The Gibbs-Thomson effect modifies the pressure and temperature at which clathrates occur, hence altering the depth at which they occur in the seabed. Nuclear magnetic resonance (NMR) measurements as a function of temperature are being conducted for water/ice/hydrate systems in a range of pore geometries, including templated SBA-15 silicas, controlled pore glasses and sol-gel silicas. Rotator-phase plastic ice is shown to be present in confined geometry, and bulk tetrahydrofuran hydrate is also shown to probably have a rotator phase. A novel NMR cryoporometry protocol, which probes both melting and freezing events while avoiding the usual problem of supercooling for the freezing event, has been developed. This enables a detailed probing of the system for a given pore size and geometry and the exploration of differences between hydrate formation and dissociation processes inside pores. These process differences have an important effect on the environment, as they impact on the ability of a marine hydrate system to re-form once warmed above a critical temperature. Ab initio quantum-mechanical molecular dynamics calculations are also being employed to probe the dynamics of liquids in pores at nanometric dimensions.

  4. Synthesis of Fluorite (CaF2 Crystal from Gypsum Waste of Phosphoric Acid Factory in Silica Gel

    Directory of Open Access Journals (Sweden)

    Mohammad Misbah Khunur

    2012-06-01

    Full Text Available This paper report the synthesis and characterization of fluorite single crystal prepared from gypsum waste of phosphoric acid production in silica gel. Instead of its high calcium, gypsum was used to recycle the waste which was massively produces in the phosphoric acid production. The gypsum waste, the raw material of CaCl2 supernatant, was dissolved in concentrated HCl and then precipitated as calcium oxalate (CaC2O4 by addition of ammonium oxalate. The CaCl2 was obtained by dissolving the CaC2O4 with HCl 3M. The crystals were grown at room temperature in silica gel and characterized by AAS, FTIR and powder XRD. The optimum crystal growth condition, which is pH of gel, CaCl2 concentration and growth time, were investigated. The result shows that at optimum condition of pH 5.80, CaCl2 concentrations of 1.2 M, and growth time of 144 hours, colorless crystals with the longest size of 3 mm, were obtained (72.57%. Characterization of the synthesized crystal by AAS indicates that the obtained crystal has high purity. Meanwhile, analysis by FTIR spectra shows a Ca–F peak at 775 cm-1, and powder-XRD analysis confirms that the obtained crystal was fluorite (CaF2. © 2012 BCREC UNDIP. All rights reservedReceived: 11st April 2012; Revised: 4th June 2012; Accepted: 13rd June 2012[How to Cite: M.M. Khunur, A. Risdianto, S. Mutrofin, Y.P. Prananto. (2012. Synthesis of Fluorite (CaF2 Crystal from Gypsum Waste of Phosphoric Acid Factory in Silica Gel. Bulletin of Chemical Reaction Engineering & Catalysis, 7 (1: 71-77.  doi:10.9767/bcrec.7.1.3171.71-77 ][How to Link / DOI: http://dx.doi.org/10.9767/bcrec.7.1.3171.71-77 ] | View in 

  5. Synthesis of silica gel from waste glass bottles and its application for the reduction of free fatty acid (FFA) on waste cooking oil

    Science.gov (United States)

    Sudjarwo, Wisnu Arfian A.; Bee, Mei Magdayanti F.

    2017-06-01

    Synthesis of silica gel from waste glass bottles was conducted with aims to characterize the product and to analyze its application forthe reduction of free fatty acid (FFA) on waste cooking oil. Silica source taken from waste glass bottles was synthesized into silica gel by using the sol-gel method. Several types of silica gel were produced with three different weight ratios of waste glass and sodium hydroxide as an extractor. They were: 1:1, 1:2, and 1:3. The results indicated that synthesized silica possessed morphology innano-sizedranging from 85 nm to 459 nm. Adsorption performance was investigated by a batch system atthe temperature between 70°C and 110°C by a range of 10°C in an hour. Analysis of the adsorption characteristic showed that the highest efficiency value of FFA reduction of 91% was obtained by silica gel with ratiosof 1:1 (SG 1) and 1:3 (SG 3). Their performances were also followed by the decline of the refractive index and the density of waste cooking oil.

  6. Preparation and characterization of quercetin-loaded silica microspheres stabilized by combined multiple emulsion and sol-gel processes

    Directory of Open Access Journals (Sweden)

    Kim Young Ho

    2015-01-01

    Full Text Available Despite exhibiting a wide spectrum of cosmeceutical properties, flavonoids and related compounds have some limitations related to their stability and solubility in distilledwater. In this project, we prepared silica microspheres using a novel method that uses polyol-in-oil-in-water (P/O/W emulsion and sol-gel methods as techniques for stabilizing quercetin. A stable microsphere suspension was successfully preparedusing a mixed solvent system comprising a polyol-phase medium for performing the sol-gel processing of tetraethyl orthosilicate (TEOS as an inorganic precursor with outer water phase. The morphology of the microsphere was evaluated using a scanning electron microscope (SEM, which showed a characteristic spherical particle shape with a smooth surface. Furthermore, SEM/EDSanalysis of a representative microsphere demonstrated that the inner structure of the silica microspheres was filled with quercetin. The mean diameter of the microsphere was in the range 20.6-35.0 μm, and the encapsulation efficiency ranged from 17.8% to 27.5%. The free and encapsulated quercetin samples were incubated in separateaqueous solutions at 25 and 42°C for 28 days. The residualcontent of the quercetin encapsulated by silica microspheres was 82% at 42°C. In contrast, that of the free quercetin stored at 42°C decreased to ~24%.

  7. Relationship between sol-gel conditions and enzyme stability: a case study with β-galactosidase/silica biocatalyst for whey hydrolysis.

    Science.gov (United States)

    Escobar, Sindy; Bernal, Claudia; Mesa, Monica

    2015-01-01

    The sol-gel process has been very useful for preparing active and stable biocatalysts, with the possibility of being reused. Especially those based on silica are well known. However, the study of the enzyme behavior during this process is not well understood until now and more, if the surfactant is involved in the synthesis mixture. This work is devoted to the encapsulation of β-galactosidase from Bacillus circulans in silica by sol-gel process, assisted by non-ionic Triton X-100 surfactant. The correlation between enzyme activity results for the β-galactosidase in three different environments (soluble in buffered aqueous reference solution, in the silica sol, and entrapment on the silica matrix) explains the enzyme behavior under stress conditions offered by the silica sol composition and gelation conditions. A stable β-galactosidase/silica biocatalyst is obtained using sodium silicate, which is a cheap source of silica, in the presence of non-ionic Triton X-100, which avoids the enzyme deactivation, even at 40 °C. The obtained biocatalyst is used in the whey hydrolysis for obtaining high value products from this waste. The preservation of the enzyme stability, which is one of the most important challenges on the enzyme immobilization through the silica sol-gel, is achieved in this study.

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

    Science.gov (United States)

    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.

  9. Substrate integrated Lead-Carbon hybrid ultracapacitor with flooded, absorbent glass mat and silica-gel electrolyte configurations

    Indian Academy of Sciences (India)

    A Banerjee; M K Ravikumar; A Jalajakshi; P Suresh Kumar; S A Gaffoor; A K Shukla

    2012-07-01

    Lead-Carbon hybrid ultracapacitors (Pb-C HUCs) with flooded, absorbent-glass-mat (AGM) and silica-gel sulphuric acid electrolyte configurations are developed and performance tested. Pb-C HUCs comprise substrate-integrated PbO2 (SI-PbO2) as positive electrodes and high surface-area carbon with graphite-sheet substrate as negative electrodes. The electrode and silica-gel electrolyte materials are characterized by XRD, XPS, SEM, TEM, Rheometry, BET surface area, and FTIR spectroscopy in conjunction with electrochemistry. Electrochemical performance of SI-PbO2 and carbon electrodes is studied using cyclic voltammetry with constant-current charge and discharge techniques by assembling symmetric electrical-double-layer capacitors and hybrid Pb-C HUCs with a dynamic Pb(porous)/PbSO4 reference electrode. The specific capacitance values for 2 V Pb-C HUCs are found to be 166 F/g, 102 F/g and 152 F/g with a faradaic efficiency of 98%, 92% and 88% for flooded, AGM and gel configurations, respectively.

  10. Silica gel microspheres decorated with covalent triazine-based frameworks as an improved stationary phase for high performance liquid chromatography.

    Science.gov (United States)

    Zhao, Wenjie; Hu, Kai; Hu, Chenchen; Wang, Xiaoyu; Yu, Ajuan; Zhang, Shusheng

    2017-03-03

    A new stationary phase for high performance liquid chromatography (HPLC) applications based on silica gel microspheres decorated with covalent triazine-based frameworks (CTF-SiO2) composite has been reported here. In this new hybrid material, sheet-like covalent triazine-based frameworks (CTF) were grown onto the supporting silica spheres, in order to achieve improved chromatographic separation and selectivity. The new material was characterized by infrared spectroscopy, elemental analysis and thermogravimetric analysis. The chromatographic performance and retention mechanism of the new stationary phase were investigated in reversed-phase mode and compared against standard C18 and cyano-modified silica (CN-SiO2) columns. A variety of different probe molecules were analyzed, including mono-substituted benzenes, polycyclic aromatic hydrocarbons, phenols, anilines and bases. The synergism of triazine and aromatic moieties provided several different retention mechanisms, thus improving the selectivity in the CTF-SiO2 composite. The good column packing properties of the uniform silica microspheres combined with the separation ability of the CTF frameworks make the new CTF-SiO2 material a potentially useful stationary phase for the analysis of complex samples.

  11. Effect of Catalyst on the Formation of Silica Coating on Nickel Substrate by Sol-Gel Processing

    Institute of Scientific and Technical Information of China (English)

    AliGhasemi; F.Ashrafizadeh; M.A.Golozar; AliAshrafi

    2004-01-01

    In this research work silica coating was produced on nickel substrates by a sol-gel process. In order to increase the rate of hydrolysis and to reduce the rate of polymerization several acid catalysts including nitric acid-hydrochloric acid, acetic acid, hydrochloric acid and nitric acid were add to silica sol. Conversely, in order to control the rate of hydrolysis and to increase the rate of polymerization, basic catalyst of ammonia and ammonia hydroxyl were introduced in to the solution. Nickel specimens of known surface roughness were chemically cleaned and prepared by dipping in the sols. In order to produce a suitable silica coating the drying and firing cycles were optimized on these substrates. The structure and uniformity of the coatings produced were examined by scanning electron microscopy. Coatings composition was determined using glow discharge optical spectroscopy and EDAX microanalysis. Experimental result showed that hydrochloric acid, acetic acid, ammonia and acetic acid-ammonia are suitable catalytic agents for silica coating formation on nickel type substrate.

  12. Nanostructuring an erbium local environment inside sol-gel silica glasses: toward efficient erbium optical fiber lasers

    Science.gov (United States)

    Savelii, Inna; El Hamzaoui, Hicham; Bigot, Laurent; Bouwmans, Géraud; Fsaifes, Ihsan; Capoen, Bruno; Bouazaoui, Mohamed

    2016-02-01

    To extend the use of erbium- (Er-)/aluminum- (Al-) codoped optical fibers in hostile environments, the reduction of the Al amount has been identified as a serious way to harden them against harsh radiation. In this work, sol-gel monolithic Er3+-doped and Er3+/Al3+-codoped silica glasses were prepared from nanoporous silica xerogels soaked in a solution containing an Er salt together or not with an Al salt. After sintering, these glasses were used as the core material of microstructured optical fibers made by the stack-and-draw method. The influence of Al incorporation on the optical properties of Er3+-doped silica glasses and fibers is investigated. This approach enabled the preparation of silica glasses containing dispersed Er3+ ions with low Al content. The obtained fibers have been tested in an all-fibered cavity laser architecture. The Er3+/Al3+-codoped fiber laser presents a maximum efficiency of 27% at 1530 nm. We show that without Al doping, the laser exhibits lower performances that depend on Er content inside the doped fiber core. The effect of Er pair-induced quenching also has been investigated through nonsaturable absorption experiments, which clearly indicate that the fraction of Er ion pairs is significantly reduced in the Al-codoped fiber.

  13. Determination of Copper in Different Ethanolic Matrices Using a Chloropropyl Silica Gel Modified with a Nanostructured Cubic Octa(3-aminopropyloctasilsesquioxane

    Directory of Open Access Journals (Sweden)

    Devaney Ribeiro Do Carmo

    2013-01-01

    Full Text Available The chloropropyl silica gel was modified with octa(3-aminopropyloctasilsesquioxane and characterized by Fourier transform infrared (FTIR spectroscopy, nuclear magnetic resonance (NMR, spectroscopies, and surface and area porosity. The specific sorption capacity of metallic ions (Cu2+ and Ni2+ increases in the following solvent order: water < ethanol 42% < ethanol < ketone. The high values of the constant (K in the order of 103 L mol−1 suggested the high adsorbent capacity of the modified silica (SGAPC for Cu2+ and Ni2+. SGAPC was applied to a separation column and shows recoveries of around 100% of copper in samples of sugar cane spirit, vodka, ginger brandy, and ethanol fuel.

  14. Adjustable rheology of fumed silica dispersion in urethane prepolymers: Composition-dependent sol and gel behaviors and energy-mediated shear responses

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, Zhong, E-mail: 11329038@zju.edu.cn; Song, Yihu, E-mail: s-yh0411@zju.edu.cn; Wang, Xiang, E-mail: 11229036@zju.edu.cn; Zheng, Qiang, E-mail: zhengqiang@zju.edu.cn [MOE Key Laboratory of Macromolecule Synthesis and Functionalization, Department of Polymer Science and Engineering, Zhejiang University, Hangzhou 310027 (China)

    2015-07-15

    Variation of colloidal and interfacial interactions leads to a microstructural diversity in fumed silica dispersions exhibiting absolutely different sol- or gel-like rheological responses. In this study, fumed silicas with different surface areas (200–400 m{sup 2}/g) and surface characteristics (hydrophilic or hydrophobic) are dispersed into moisture-cured polyurethane. The microstructures investigated using transmission electron microscope are associated perfectly with three different rheological behaviors: (i) Sols with well-dispersed silica aggregates, (ii) weak gels with agglomerate-linked networks, and (iii) strong gels with concentrated networks of large agglomerates. Though sols and gels are well distinguished by shear thickening or sustained thinning response through steady shear flow test, it is interesting that the sols and weak gels exhibit a uniform modulus plateau-softening-hardening-softening response with increasing dynamic strain at frequency 10 rad s{sup −1} while the strong gels show a sustained softening beyond the linear regime. Furthermore, the onset of softening and hardening can be normalized: The two softening are isoenergetic at mechanical energies of 0.3 J m{sup −3} and 10 kJ m{sup −3}. On the other hand, the hardening is initiated by a critical strain of 60%. The mechanisms involved in the generation of the sol- and the gel-like dispersions and their structural evolutions during shear are thoroughly clarified in relation to the polyols, the characteristic and content of silica and the curing catalysts.

  15. Determination of picomolar beryllium levels in seawater with inductively coupled plasma mass spectrometry following silica-gel preconcentration

    Energy Technology Data Exchange (ETDEWEB)

    Tazoe, Hirofumi, E-mail: tazoe@cc.hirosaki-u.ac.jp [Department of Radiation Chemistry, Institute of Radiation Emergency Mediation, Hirosaki University, 66-1 Hon-cho, Hirosaki, Aomori 036-8564 (Japan); College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan); Yamagata, Takeyasu [College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan); Obata, Hajime [Atmosphere and Ocean Research Institute, The Tokyo University, 5-1-5 Kashiwanoha, Kashiwa-shi, Chiba 277-8564 (Japan); Nagai, Hisao [College of Humanities and Sciences, Nihon University, 3-25-40, Sakurajosui, Setagaya-ku, Tokyo 156-8550 (Japan)

    2014-12-10

    Highlights: • We developesd the simplest and robust SPE method for ultra low picomolar level beryllium in seawater. • Just silica gel column can quantitatively adsorb beryllium in neutral pH condition containing natural seawater. • EDTA solution can eliminate seawater matrixes retaining Be in the column, which optimize to ICP-MS detemination. • Accurate and precise Be data have been obtained for natural seawater from North Pacific Ocean. - Abstract: A robust and rapid method for the determination of natural levels of beryllium (Be) in seawater was developed to facilitate mapping Be concentrations in the ocean. A solid-phase extraction method using a silica gel column was applied for preconcentration and purification of Be in seawater prior to determination of Be concentrations with inductively coupled plasma mass spectrometry (ICP-MS). Be was quantitatively adsorbed onto silica gel from solutions with pH values ranging from 6.3 to 9, including natural seawater. The chelating agent ethylenediamine tetraacetic acid was used to remove other ions in the seawater matrix (Na, Mg, and Ca) that interfere with the ICP-MS analysis. The reproducibility of the method was 3% based on triplicate analyses of natural seawater samples, and the detection limit was 0.4 pmol kg{sup −1} for 250 mL of seawater, which is sufficient for the analysis of seawater in the open ocean. The method was then used to determine the vertical profile of Be in the eastern North Pacific Ocean, which was found to be a recycled-type profile in which the Be concentration increased with depth from the surface (7.2 pmol kg{sup −1} at <200 m) to deep water (29.2 pmol kg{sup −1} from 3500 m to the bottom)

  16. Synthesis and characterization of sol–gel derived ZnS : Mn2+ nanocrystallites embedded in a silica matrix

    Indian Academy of Sciences (India)

    B Bhattacharjee; D Ganguli; K Iakoubovskii; A Stesmans; S Chaudhuri

    2002-06-01

    Synthesis and characterization of undoped and Mn2+ doped ZnS nanocrystallites (radius 2–3 nm) embedded in a partially densified silica gel matrix are presented. Optical transmittance, photoluminescence (PL), ellipsometric and electron spin resonance measurements revealed manifestation of quantum size effect. PL spectra recorded at room temperature revealed broad blue emission signal centred at ∼ 420 nm and Mn2+ related yellow–orange band centred at ∼ 590 nm while ESR indicated that Mn in ZnS was present as dispersed impurity rather than Mn cluster.

  17. Efficient and reversible CO2 capture by amine functionalized-silica gel confined task-specific ionic liquid system

    OpenAIRE

    Javad Aboudi; Majid Vafaeezadeh

    2015-01-01

    Simple, efficient and practical CO2 capture method is reported using task-specific ionic liquid (IL) supported onto the amine-functionalized silica gel. The results have been shown that both the capacity and rate of the CO2 absorption notably increase in the supported IL/molecular sieve 4 Å system in comparison of homogeneous IL. Additionally, it has shown that the prepared material is capable for reversible carbon dioxide absorption for at least 10 cycles without significant loss of efficien...

  18. Silica gel modified with ethylenediamine and succinic acid-adsorption and calorimetry of cations in aqueous solution

    Energy Technology Data Exchange (ETDEWEB)

    Arakaki, L.N.H.; Filha, V.L.S. Augusto; Germano, A.F.S.; Santos, S.S.G. [Department of Chemistry, Federal University of Paraíba, 58051-900 João Pessoa, Paraíba (Brazil); Fonseca, M.G., E-mail: mgardennia@quimica.ufpb.br [Department of Chemistry, Federal University of Paraíba, 58051-900 João Pessoa, Paraíba (Brazil); Sousa, K.S.; Espínola, J.G.P. [Department of Chemistry, Federal University of Paraíba, 58051-900 João Pessoa, Paraíba (Brazil); Arakaki, T. [Department of Food Engineering, CT, Federal University of Paraíba, 58059-900 João Pessoa, Paraíba (Brazil)

    2013-03-20

    Highlights: ► Succinic acid-modified silica acted as an adsorbent for Cu (II), Ni (II), and Co (II) from aqueous solutions. ► Modified silica adsorbed metallic cations in the order Cu{sup 2+} > Co{sup 2+} > Ni{sup 2+}. ► Succinic acid-modified silica could be employed as low-cost material for the removal of cations from aqueous solution. ► Thermodynamic data for these systems are favorable at the solid/liquid interface. - Abstract: Ethylenediamine molecules were covalently immobilized onto silica gel previously functionalized with 3-chlorosilylpropyltrimethoxysilane (Sil–Cl), producing a Sil–N surface. The Sil–N surface reacted with succinic acid, yielding a Sil–NSuc surface. This new synthesized silica gel surface was used to adsorb divalent cations from aqueous solutions at room temperature. The adsorption isotherms were fit to a modified Langmuir equation using the data obtained by suspending the solid in MCl{sub 2} (M = Cu, Ni, and Co) aqueous solutions, yielding the maximum number of moles adsorbed as 1.04 ± 0.01, 1.89 ± 0.02 and 1.85 ± 0.02 mmol g{sup −1} for divalent copper, nickel and cobalt, respectively. The metal-basic center ratio for complexes on the surfaces varied with the nature of the metal. The spontaneity of these systems was reflected in the negative values of the Gibbs free energy calculated using calorimetric data. The net thermal effects obtained from the calorimetric titration measurements were adjusted to a modified Langmuir equation, and the calculation of the enthalpies of the interaction for the complexation with Sil–NSuc yielded the following exothermic values: 2.81 ± 0.08, 0.35 ± 0.04 ± and 0.69 ± 0.05 kJ mol{sup −1} for Cu{sup 2+}, Co{sup 2+} and Ni{sup 2+}, respectively. Based on these values, the metals are preferentially adsorbed in the order Cu{sup 2+} > Co{sup 2+} > Ni{sup 2+}. The other thermodynamic data for these systems are favorable at the solid/liquid interface, suggesting the efficacy of this

  19. Gold nanoparticles grafted modified silica gel as a new stationary phase for separation and determination of steroid hormones by thin layer chromatography

    Directory of Open Access Journals (Sweden)

    Mitra Amoli-Diva

    2015-06-01

    Full Text Available A new thin layer chromatographic layer using gold nanoparticles grafted 3-triethoxysilyl propylamine modified silica gel (Au NPs-APTS modified silica gel was developed as a stationary phase for separation and determination of two steroid hormones, namely progesterone and testosterone. Acetone–n-hexane 25:75 (v/v was used as the mobile phase, and the results were compared with those obtained using plain (i.e., unmodified silica gel plates. Some chromatographic parameters used for separation of the two steroids on an Au NPs-APTS modified silica gel plate as well as on a plain silica gel plate, including ΔRF, separation factor (α, and resolution (RS, were evaluated and compared. The reproducibility of RF values was also determined by analysis of the two steroids in 7 consecutive days on both plates. Validity of the method was investigated, and a wide linear range of 1–200 ng per spot, and low detection limits of 0.16 ng and 0.13 ng per spot, low quantification limits of 0.51 ng and 0.40 ng per spot, and good precision (expressed as percent relative standard deviation lower than 3.1% and 2.7% were obtained for progesterone and testosterone, respectively. As the results revealed, the proposed method is rapid and sensitive, and it is applicable to separation and determination of progesterone and testosterone in biological matrices such as urine samples.

  20. Preparation of silane-functionalized silica films via two-step dip coating sol–gel and evaluation of their superhydrophobic properties

    Energy Technology Data Exchange (ETDEWEB)

    Ramezani, Maedeh, E-mail: m.ramezani@merc.ac.ir [Division of Nanotechnology and Advanced Materials, Materials and Energy Research Center, P.O. Box 31787-316, Karaj (Iran, Islamic Republic of); Vaezi, Mohammad Reza [Division of Nanotechnology and Advanced Materials, Materials and Energy Research Center, P.O. Box 31787-316, Karaj (Iran, Islamic Republic of); Kazemzadeh, Asghar [Division of Semiconductors, Materials and Energy Research Center, P.O. Box 31787-316, Karaj (Iran, Islamic Republic of)

    2014-10-30

    Highlights: • Superhydrophobic silica film was prepared by sol–gel process. • The surfaces exhibited superhydrophobicity with water contact angle greater than 150°. • AFM images showed the roughness increases with increasing the percentage of silylation agent. • Before and after modification, the particle size of silica was lower than 50 nm. - Graphical abstract: Schematic illustration of the surface modification of the silica nanoparticle by iso-OTMS on the glass substrate. - Abstract: In this paper, we study the two-step dip coating via a sol–gel process to prepare superhydrophobic silica films on the glass substrate. The water repellency of the silica films was controlled by surface silylation method using isooctyltrimethoxysilane (iso-OTMS) as a surface modifying agent. Silica alcosol was synthesized by keeping the molar ratio of ethyltriethoxysilane (ETES) precursor, ethanol (EtOH) solvent, water (H{sub 2}O) was kept constant at 1:36:6.6 respectively, with 6 M NH{sub 4}OH throughout the experiment and the percentages of hydrophobic agent in hexane bath was varied from 0 to 15 vol.%. The static water contact angle values of the silica films increased from 108° to 160° with an increase in the vol.% of iso-OTMS. At 15 vol%. of iso-OTMS, the silica film shows static water contact angle as high as 160°. The superhydrophobic silica films are thermally stable up to 440 °C and above this temperature, the silica films lose superhydrophobicity. By controlling the primer particle size of SiO{sub 2} about 26 nm, leading to decrease the final size of silica nanoparticles after modification of nanoparticles by isooctyltrimethoxysilane about 42 nm. The films are transparent and have uniform size on the surface. The silica films have been characterized by atomic force microscopy (AFM), fourier transform infrared spectroscopy (FT-IR), transparency, contact angle measurement (CA), Zeta-potential, Thermal stability by TG–DTA analysis.

  1. In-situ growth and spectrum characterization of ZnSe nanocrystals in silica gel-glasses

    Institute of Scientific and Technical Information of China (English)

    WANG Minqiang; WANG Yunpeng; YAO Xi; KONG Fantao; ZHANG Liangying

    2004-01-01

    ZnSe nanocrystals were in-situ grown in silica gel-glasses by using sol-gel process and the reductive thermal treatment. The transparent, homogeneous ZnSe/SiO2 nanocomposites with the yellow color were first obtained. We used X-ray diffraction pattern (XRD), UV-VIS optical absorption and Raman scattering to characterize the spectrum properties of ZnSe nanocrystals. The broadening of XRD peaks, the blueshift of interband optical absorption edge and the change of Raman spectrum were observed. From these experimental results, we theoretically calculated the size of ZnSe nanocrystals. The results of XRD, optical absorption and Raman spectra were approximately consistent, with the mean diameter of about 4.6 nm. The discrepancies from different methods were discussed.

  2. Ceria nanoparticles vis-à-vis cerium nitrate as corrosion inhibitors for silica-alumina hybrid sol-gel coating

    Science.gov (United States)

    Lakshmi, R. V.; Aruna, S. T.; Sampath, S.

    2017-01-01

    The present work provides a comparative study on the corrosion protection efficiency of defect free sol-gel hybrid coating containing ceria nanoparticles and cerium nitrate ions as corrosion inhibitors. Less explored organically modified alumina-silica hybrid sol-gel coatings are synthesized from 3-glycidoxypropyltrimethoxysilane and aluminium-tri-sec-butoxide. The microemulsion derived nanoparticles and the hybrid coatings are characterized and compared with coatings containing cerium nitrate. Corrosion inhibiting capability is assessed using electrochemical impedance spectroscopy. Scanning Kelvin probe measurements are also conducted on the coatings for identifying the apparent corrosion prone regions. Detailed X-ray photoelectron spectroscopy (XPS) analysis is carried out to comprehend the bonding and corrosion protection rendered by the hybrid coatings.

  3. Silica- and germania-based dual-ligand sol-gel organic-inorganic hybrid sorbents combining superhydrophobicity and π-π interaction. The role of inorganic substrate in sol-gel capillary microextraction.

    Science.gov (United States)

    Seyyal, Emre; Malik, Abdul

    2017-04-29

    Principles of sol-gel chemistry were utilized to create silica- and germania-based dual-ligand surface-bonded sol-gel coatings providing enhanced performance in capillary microextraction (CME) through a combination of ligand superhydrophobicity and π-π interaction. These organic-inorganic hybrid coatings were prepared using sol-gel precursors with bonded perfluorododecyl (PF-C12) and phenethyl (PhE) ligands. Here, the ability of the PF-C12 ligand to provide enhanced hydrophobic interaction was advantageously combined with π-π interaction capability of the PhE moiety to attain the desired sorbent performance in CME. The effect of the inorganic sorbent component on microextraction performance of was explored by comparing microextraction characteristics of silica- and germania-based sol-gel sorbents. The germania-based dual-ligand sol-gel sorbent demonstrated superior CME performance compared to its silica-based counterpart. Thermogravimetric analysis (TGA) of the created silica- and germania-based dual-ligand sol-gel sorbents suggested higher carbon loading on the germania-based sorbent. This might be indicative of more effective condensation of the organic ligand-bearing sol-gel-active chemical species to the germania-based sol-gel network (than to its silica-based counterpart) evolving in the sol solution. The type and concentration of the organic ligands were varied in the sol-gel sorbents to fine-tune extraction selectivity toward different classes of analytes. Specific extraction (SE) values were used for an objective comparison of the prepared sol-gel CME sorbents. The sorbents with higher content of PF-C12 showed remarkable affinity for aliphatic hydrocarbons. Compared to their single-ligand sol-gel counterparts, the dual-ligand sol-gel coatings demonstrated significantly superior CME performance in the extraction of alkylbenzenes, providing up to ∼65.0% higher SE values. The prepared sol-gel CME coatings provided low ng L(-1) limit of detections (LOD

  4. Thin layer chromatographic separation of cobalt from nickel on impregnated silica gel layers:quantitative determination by digital image analysis%Thin layer chromatographic separation of cobalt from nickel on impregnated silica gel layers: quantitative determination by digital image analysis

    Institute of Scientific and Technical Information of China (English)

    P A MOHAMED NAJAR; R G SONALI; M T NIMJE; K V RAMANA RAO

    2012-01-01

    Thin layer chromatography (TLC) of cobalt and nickel has been performed on silica gel layers induced with alkali mediated cellulose extract.A novel combination of 10% aqueous solutions of Tween-20 and potassium thiocyanate in 1∶ 1 (v/v) was identified as the best mobile phase for the selective separation of Co2+ from Ni2+ on the impregnated Silica Gel G layers.The chromatographic characteristics of the cations were studied and the limits of detection as well as the limits of quantification for Co2+ and Ni2+ were determined.The quantitative estimation of the cations was achieved from the digital image analysis of respective chromatograms.The proposed quantitative method was successfully applied with 0-0.50% error for the determination of Co2+ from Ni2+ in spiked samples of bauxite,soil and rock containing common cations such as Al3+,Fe2+,Ti4+,Zn2+,Mn2+,Cu2+,Cr6+,Mg2+ etc.under the optimized chromatographic conditions.

  5. Catalytic activity of acid and base with different concentration on sol-gel kinetics of silica by ultrasonic method.

    Science.gov (United States)

    Das, R K; Das, M

    2015-09-01

    The effects of both acid (acetic acid) and base (ammonia) catalysts in varying on the sol-gel synthesis of SiO2 nanoparticles using tetra ethyl ortho silicate (TEOS) as a precursor was determined by ultrasonic method. The ultrasonic velocity was received by pulsar receiver. The ultrasonic velocity in the sol and the parameter ΔT (time difference between the original pulse and first back wall echo of the sol) was varied with time of gelation. The graphs of ln[ln1/ΔT] vs ln(t), indicate two region - nonlinear region and a linear region. The time corresponds to the point at which the non-linear region change to linear region is considered as gel time for the respective solutions. Gelation time is found to be dependent on the concentration and types of catalyst and is found from the graphs based on Avrami equation. The rate of condensation is found to be faster for base catalyst. The gelation process was also characterized by viscosity measurement. Normal sol-gel process was also carried out along with the ultrasonic one to compare the effectiveness of ultrasonic. The silica gel was calcined and the powdered sample was characterized with scanning electron microscopy, energy dispersive spectra, X-ray diffractogram, and FTIR spectroscopy.

  6. Silica-gel structural characterization during the initial phases of gelation and drying; Caracterizacao estrutural de geis de silica durante as etapas iniciais de gelacao e secagem

    Energy Technology Data Exchange (ETDEWEB)

    Ferreira, Max Passos

    1996-12-31

    For centuries, glasses and ceramics have been made via melting or solid state reactions at temperatures above 100 deg C. The sol-gel process offers new approaches to the synthesis of glasses and ceramics, combining control of composition and structure at the molecular level with the ability to shape materials in bulk, powder, fiber and thin-film forms. The growth of sol-gel technology research is due to the many unique features of that class of materials. Major applications include optical elements and integrated optical devices, ceramic filters, membranes, supercondutors, magnetic, catalytic and manostructured materials to antioxidant, anticorrosion coatings and composite and biomedical materials. In this work a variety of techniques like spectroscopy, Raman spectroscopy, ultraviolet-visible spectroscopy, light scattering nuclear magnetic resonance, X ray diffraction and nitrogen adsorption have been employed to investigate the initial phase of the sol-gel transition of gamma ray irradiated tetramethoxysilane (TMOS) solutions and non-irradiated TMOS solution and to get information about the structure of the silica gels obtained under different gelation conditions. Typically the tetramethoxysilane solutions were prepared using a molar ratio of TMOS to demineralized water of 1 to 16. Some experiments were made under catalysed conditions. The mixing was carried out at room temperature. The turbidity and light scattering experiments on the polycondensation of tetramethoxysilane show that exists no drastic difference in the gelling time of a gamma ray irradiated and a non-irradiated TMOS+H{sub 2}O (1+16 M) solution. In the absence of a catalyst, the gelling time for both reactions occurs in about 3.30 h. When HNO{sub 3} (o.03 M) was used, the gelling time observed was 3 days. Raman and ultraviolet-visible spectroscopy show no drastic difference during the initial phase at the sol-gel transition under ambient temperature/pressure and under gamma radiation. The gels

  7. Formation and characterization of different ceria/silica composite materials via dispersion of ceria gel or soluble ceria precursors in silica sols.

    Science.gov (United States)

    Khalil, Kamal M S; Elkabee, Leena A; Murphy, Brian

    2005-07-15

    Composite ceria/silica materials of 10 and 20% (w/w) were prepared by calcination, at 650 degrees C for 3 h, of the xerogels obtained by mixing the corresponding amount of a ceria precursor with freshly prepared sols of spherical silica particles (Stober particles) in their mother liquors. Two different ceria precursors were examined in this investigation. The first was a gel produced by the prehydrolysis of cerium(IV) isopropoxide in isopropanol medium, and the second was an aqueous solution of cerium(IV) ammonium nitrate. Different textural and morphological characteristics that developed by calcination were investigated by TGA, FTIR, XRD, SEM, and analyses of N2 adsorption isotherms. The results indicated that ceria dispersion and formation of mesoporous textural composite materials produced by the second precursor, cerium(IV) ammonium nitrate, are better than those produced by the first precursor, prehydrolyzed cerium(IV) isopropoxide. The results are discussed in terms of the effect of precursors and mixing media on nucleation and growth of ceria particles and their protection from sintering on calcination at the test temperature.

  8. Molecular characterization of gel and liquid-crystalline structures of fully hydrated POPC and POPE bilayers.

    Science.gov (United States)

    Leekumjorn, Sukit; Sum, Amadeu K

    2007-05-31

    Molecular dynamics simulations were used for a comprehensive study of the structural properties of monounsaturated POPC and POPE bilayers in the gel and liquid-crystalline state at a number of temperatures, ranging from 250 to 330 K. Though the chemical structures of POPC and POPE are largely similar (choline versus ethanolamine headgroup), their transformation processes from a gel to a liquid-crystalline state are contrasting. In the similarities, the lipid tails for both systems are tilted below the phase transition and become more random above the phase transition temperature. The average area per lipid and bilayer thickness were found less sensitive to phase transition changes as the unsaturated tails are able to buffer reordering of the bilayer structure, as observed from hysteresis loops in annealing simulations. For POPC, changes in the structural properties such as the lipid tail order parameter, hydrocarbon trans-gauche isomerization, lipid tail tilt-angle, and level of interdigitation identified a phase transition at about 270 K. For POPE, three temperature ranges were identified, in which the lower one (270-280 K) was associated with a pre-transition state and the higher (290-300 K) with the post-transition state. In the pre-transition state, there was a significant increase in the number of gauche arrangements formed along the lipid tails. Near the main transition (280-290 K), there was a lowering of the lipid order parameters and a disappearance of the tilted lipid arrangement. In the post-transition state, the carbon atoms along the lipid tails became less hindered as their density profiles showed uniform distributions. This study also demonstrates that atomistic simulations of current lipid force fields are capable of capturing the phase transition behavior of lipid bilayers, providing a rich set of molecular and structural information at and near the main transition state.

  9. Direct analysis of silica gel extracts from immunostained glycosphingolipids by nanoelectrospray ionization quadrupole time-of-flight mass spectrometry.

    Science.gov (United States)

    Meisen, Iris; Peter-Katalinić, Jasna; Müthing, Johannes

    2004-04-15

    A combined strategy of preparative high-performance thin-layer chromatography overlay assay and mass spectrometry was established for the structural characterization of immunostained glycosphingolipids (GSLs) in silica gel extracts. Crude chloroform/methanol/water (30/60/8, v/v/v) extracts of immunostained TLC bands were analyzed by nanoelectrospray low-energy CID mass spectrometry without further purification. The GSL species investigated were isomeric monosialogangliosides of the neolacto series from a ganglioside preparation of human granulocytes, the disialoganglioside GD3 from a human melanoma lipid extract, and ganglio series Gg3Cer of a neutral GSL preparation from murine lymphoreticular MDAY-D2 cells. For the specific detection of lipid-bound oligosaccharides, polyclonal chicken IgY, murine monoclonal IgG3, and IgM antibodies were used. The resulting mass spectra show that only analytical quantities of approximately 1 microg of a single GSL within a complex mixture are required for the structure determination of immunostained GSLs by MS and MS/MS. All species investigated were detected as singly charged deprotonated molecular ions, and neither buffer-derived salt adducts nor coextracted contaminants from the immunostaining procedure or the silica gel layer were observed. This effective HPTLC-MS-joined procedure offers a wide range of applications for any carbohydrate binding agents such as bacterial toxins, plant lectins, and others.

  10. A Thermally Conductive Composite with a Silica Gel Matrix and Carbon-Encapsulated Copper Nanoparticles as Filler

    Science.gov (United States)

    Lin, Jin; Zhang, Haiyan; Hong, Haoqun; Liu, Hui; Zhang, Xiubin

    2014-07-01

    Core-shell-structured nanocapsules with a copper core encapsulated in a carbon shell (Cu-C) were synthesized by a direct-current arc-discharge method. Morphological and microstructural characterization showed that the Cu-C consisted of a nanosized Cu core and carbon shell, with the carbon shells containing 6 to 15 ordered graphitic layers and amorphous carbon that effectively shield the metallic Cu core from oxidation. A thermally conductive composite was successfully fabricated using a silica gel matrix incorporated with Cu-C filler. The Cu-C nanoparticles were homogeneously dispersed in the silica gel. The effects of Cu-C on the thermal conductivity, electrical resistivity, and coefficient of thermal expansion (CTE) of the composite were investigated. For composites with 6.16 vol.%, 11.04 vol.%, 16.70 vol.%, and 23.34 vol.% Cu-C content, the thermal conductivity at 50°C was 0.32 W/(m K) to 0.77 W/(m K), the electrical resistivity was 1.98 × 109, 3.48 × 107, 302, and 1 Ω m, respectively, while the CTE at 200°C was 3.79 × 10-4 K-1 to 3.44 × 10-4 K-1. The results reveal that the ordered graphitic shells in the Cu-C increased both the thermal and electrical conduction, but decreased the CTE by preventing the Cu cores from expanding.

  11. Selective speciation of inorganic antimony on tetraethylenepentamine bonded silica gel column and its determination by graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Mendil, Durali; Bardak, Hilmi; Tuzen, Mustafa; Soylak, Mustafa

    2013-03-30

    A speciation system for antimony (III) and antimony (V) ions that based on solid phase extraction on tetraethylenepentamine bonded silica gel has been established. Antimony was determined by graphite furnace atomic absorption spectrometry (GF-AAS). Analytical conditions including pH, sample volume, etc., were studied for the quantitative recoveries of Sb (III) and Sb (V). Matrix effects on the recovery were also investigated. The recovery values and detection limit for antimony (III) at optimal conditions were found as >95% and 0.020 μg L(-1), respectively. Preconcentration factor was calculated as 50. The capacity of adsorption for the tetraethylenepentamine bonded silica gel was 7.9 mg g(-1). The validation was checked by analysis of NIST SRM 1573a Tomato laves and GBW 07605 Tea certified reference materials. The procedure was successfully applied to speciation of antimony in tap water, mineral water and spring water samples. Total antimony was determined in refined salt, unrefined salt, black tea, rice, tuna fish and soil samples after microwave digestion and presented enrichment method combination. Copyright © 2013 Elsevier B.V. All rights reserved.

  12. Catechol functionalized aminopropyl silica gel: synthesis, characterization and preconcentrative separation of uranium(VI) from thorium(IV)

    Energy Technology Data Exchange (ETDEWEB)

    Metilda, P.; Mary Gladis, J.; Prasada Rao, T.P. [Regional Research Lab. (CSIR), Trivandrum (India)

    2005-07-01

    A novel solid phase extractant is prepared by chemically immobilizing catechol with diazotized aminopropyl silica gel. The resulting catechol functionalized silica gel (CASG) was characterized by FTIR, and microanalysis and was used for selective enrichment of uranium(VI) from other inorganic ions. The optimum pH range for maximum sorption of uranium(VI) and thorium(IV) was found to be in the range 3.5-6.0. The above actinides were eluted with 10 cm{sup 3} of 1.0 mol dm{sup -3} HCl and determined by using an Arsenazo III spectrophotometric procedure. The calibration graph was rectilinear over the uranium(VI) concentration in the range 2-100 {mu}g dm{sup -3} with a relative standard deviation of 2.15% (for 25 {mu}g of uranium(VI) present in 1.0 dm{sup 3} of sample). The validation of the developed preconcentration procedure was carried out by analyzing marine sediment (MESS-3, NRC, Canada) and soil (IAEA soil-7, Austria) reference materials. The developed preconcentration method enables a simple instruments like a spectrophotometer gave comparable values of uranium(VI) to that of standard inductively coupled plasma-mass spectrometric values during the analysis of real soil and sediment samples. (orig.)

  13. Disiloxanes and Functionalized Silica Gels: One Route, Two Complementary Outcomes-Guanidinium and Pyridinium Ion-Exchangers.

    Directory of Open Access Journals (Sweden)

    Łukasz Tabisz

    Full Text Available Five novel disiloxane compounds comprising guanidinium and pyridinium moieties were obtained with high yields and purity. The verified synthetic pathways were then applied for modification of pre-functionalized silica gel, producing materials with the analogous organic side-chains. These halide-containing compounds and materials were then compared as to their ion-exchange properties: two disiloxanes proved to be effective in leaching different anions (nitrate, benzoate and ascorbate from solid to organic phase, and pyridinium-functionalized silica gels showed selectivity towards perchlorate ion, removing it from methanolic solutions with preference to other singly charged anions. The results presented demonstrate that both compounds and materials containing silicon-carbon bonds can be produced using the same methodology, but offer strikingly different application opportunities. Comparison of their properties provides additional insight into the binding mode of different anions and hints at how the transition from a flexible siloxane bridge to immobilization on solid surface influences anion-binding selectivity. Additionally, one of the siloxane dipodands was found to form a crystalline and poorly soluble nitrate salt (1.316 g/L, water, although it was miscible with a wide range of solvents as a hydrochloride. A possible explanation is given with the help of semi-empirical calculations. A simple, time- and cost-efficient automated potentiometric titration methodology was used as a viable analytical tool for studying ion-exchange processes for both compounds and materials, in addition to standard NMR, FT-IR and ESI-MS methods.

  14. Thermal and catalytic degradation of polyethylene wastes in the presence of silica gel, 5A molecular sieve and activated carbon.

    Science.gov (United States)

    González, Yovana Sander; Costa, Carlos; Márquez, M Carmen; Ramos, Pedro

    2011-03-15

    A comparative study of thermal and catalytic degradation of polyethylene wastes has been carried out with the aim of obtaining chemical compounds with potential use in the chemical industry and the energy production. Polyethylene wastes were obtained from polyethylene bags used in supermarkets. Catalysts utilized in the study were silica gel, 5A molecular sieve and activated carbon. The pyrolysis was performed in a batch reactor at 450, 500 and 700 °C during 2h for each catalyst. The ratio catalyst/PE was 10% w/w and the solid and gaseous products were analyzed by gas chromatography and mass spectrometry. The optimum operation temperature and the influence of the three catalysts are discussed with regards to the products formed. The best temperature for degradation with silica gel and activated carbon as catalysts was 450 °C and with 5A molecular sieve was 700 °C. Degradation products of PE (solid fraction and gas fraction) are depending on temperature and catalyst used. External surface and structure of catalysts were visualized by Scanning Electron Microscopy (SEM) and the contribution on product distribution is commented. All products from different degradations could be used as feed stocks in chemical industry or in energy production based on the value of heat of combustion for solid fraction (45000 J/g), similar to the heat of combustion of commercial fuels.

  15. Low-cost and effective phenol and basic dyes trapper derived from the porous silica coated with hydrotalcite gel.

    Science.gov (United States)

    Tao, Yu Fei; Lin, Wei Gang; Gao, Ling; Yang, Jin; Zhou, Yu; Yang, Jia Yuan; Wei, Feng; Wang, Ying; Zhu, Jian Hua

    2011-06-15

    Novel low-cost and effective adsorbents of phenol and basic dyes were made by coating amorphous silica with hydrotalcite (HT) gel followed by soaking in alkaline solution, and the surface basic-acidic properties of resulting composites were evaluated by CO(2)-TPD, Hammett indicator method and NH(3)-TPD, respectively. Both BET surface area and microporous surface area of the composites were increased after they were soaked with alkaline solution; meanwhile the center of pore size distribution was changed from 9 to 3-4 nm. These composites efficiently captured phenol in gaseous and liquid phases, superior to mesoporous silica such as MCM-48 or SBA-15 and zeolite NaY, and the equilibrium data of gaseous adsorption could be well fitted to Freundlich model. These modified silicas also exhibited high adsorption capacity forward basic dyes such as crystal violet (CV) and leuco-crystal violet (LCV), reaching the adsorption equilibrium within 1 h and offering a new material for environment protection.

  16. Characteristic coordination structure around Nd Ions in sol-gel-derived Nd-Al-codoped silica glasses.

    Science.gov (United States)

    Funabiki, Fuji; Kajihara, Koichi; Kaneko, Ken; Kanamura, Kiyoshi; Hosono, Hideo

    2014-07-24

    Al codoping can improve the poor solubility of rare-earth ions in silica glasses. However, the mechanism is not well understood. The coordination structure around Nd ions in sol-gel-derived Nd-Al-codoped silica glasses with different Al content was investigated by optical and pulsed electron paramagnetic resonance spectroscopies. Both tetrahedral AlO4 and octahedral AlO6 units were observed around Nd ions as ligands. The average total number of these two types of ligands for each Nd(3+) ion was ∼ 2 irrespective of Al content and was larger by 1-2 orders of magnitude than that calculated for a uniform distribution of codopant ions (∼ 0.08-0.25). With increasing Al content, AlO4 units disappeared and AlO6 units became dominant. The preferential coordination of AlOx (x = 4, 6) units to Nd ions enabled the amount of Al necessary to dissolve Nd ions uniformly in silica glass at a relatively low temperature of 1150-1200 °C to be minimized, and the conversion of AlO4 units to AlO6 units around Nd ions caused the asymmetry of the crystal field at the Nd sites to increase and the site-to-site distribution to decrease.

  17. A bioactive coating of a silica xerogel/chitosan hybrid on titanium by a room temperature sol-gel process.

    Science.gov (United States)

    Jun, Shin-Hee; Lee, Eun-Jung; Yook, Se-Won; Kim, Hyoun-Ee; Kim, Hae-Won; Koh, Young-Hag

    2010-01-01

    A bioactive coating consisting of a silica xerogel/chitosan hybrid was applied to Ti at room temperature as a novel surface treatment for metallic implants. A crack-free thin layer (coated on Ti with a chitosan content of >30 vol.% through a sol-gel process. The coating layer became more hydrophilic with increasing silica xerogel content, as assessed by contact angle measurement. The hybrid coatings afforded excellent bone bioactivity by inducing the rapid precipitation of apatite on their surface when immersed in a simulated body fluid (SBF). Osteoblastic cells cultured on the hybrid coatings were more viable than those on a pure chitosan coating. Furthermore, the alkaline phosphate activity of the cells was significantly higher on the hybrid coatings than on a pure chitosan coating, with the highest level being achieved on the hybrid coating containing 30% chitosan. These results indicate that silica xerogel/chitosan hybrids are potentially useful as room temperature bioactive coating materials on titanium-based medical implants.

  18. Surface chemical modification of TEOS based silica aerogels synthesized by two step (acid-base) sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Bhagat, Sharad D. [Air Glass Laboratory, Department of Physics, Shivaji University, Kolhapur 416 004, Maharashtra (India); Rao, A. Venkateswara [Air Glass Laboratory, Department of Physics, Shivaji University, Kolhapur 416 004, Maharashtra (India)]. E-mail: avrao_phy@unishivaji.ac.in

    2006-04-15

    The present paper describes the comparative studies on the hydrophobic and physical properties of the tetraethoxysilane (TEOS) based silica aerogels prepared by two step sol-gel process followed by supercritical drying. Silica alcogels were prepared by keeping the molar ratio of TEOS:methanol (MeOH):H{sub 2}O (acidic):H{sub 2}O (basic) constant at 1:33:3.5:3.5 with oxalic acid and ammonium hydroxide concentrations fixed at 0.001 and 1 M, respectively. In all, nine different co-precursors (CP) of the type R {sub n}SiX{sub 4-n}, have been used. The aerogels have been characterized by density, porosity, percentage of volume shrinkage, optical transmission, contact angle and thermal conductivity measurements. The surface chemical modification of silica aerogels was confirmed by the presence of C-H and Si-C peaks at 2900, 1450 and 840 cm{sup -1}, respectively, from the Fourier transform-infrared spectroscopy (FT-IR). The microstructure of the aerogels was studied using transmission electron microscopy (TEM) and scanning electron microscopy (SEM) techniques. In addition to these studies, the stability of the hydrophobic aerogels against an organic impurity (methanol, in the present studies) in water has also been studied.

  19. Surface chemical modification of TEOS based silica aerogels synthesized by two step (acid base) sol gel process

    Science.gov (United States)

    Bhagat, Sharad D.; Rao, A. Venkateswara

    2006-04-01

    The present paper describes the comparative studies on the hydrophobic and physical properties of the tetraethoxysilane (TEOS) based silica aerogels prepared by two step sol-gel process followed by supercritical drying. Silica alcogels were prepared by keeping the molar ratio of TEOS:methanol (MeOH):H 2O (acidic):H 2O (basic) constant at 1:33:3.5:3.5 with oxalic acid and ammonium hydroxide concentrations fixed at 0.001 and 1 M, respectively. In all, nine different co-precursors (CP) of the type R nSiX 4 - n, have been used. The aerogels have been characterized by density, porosity, percentage of volume shrinkage, optical transmission, contact angle and thermal conductivity measurements. The surface chemical modification of silica aerogels was confirmed by the presence of C sbnd H and Si sbnd C peaks at 2900, 1450 and 840 cm -1, respectively, from the Fourier transform-infrared spectroscopy (FT-IR). The microstructure of the aerogels was studied using transmission electron microscopy (TEM) and scanning electron microscopy (SEM) techniques. In addition to these studies, the stability of the hydrophobic aerogels against an organic impurity (methanol, in the present studies) in water has also been studied.

  20. The influence of sol-gel-derived silica coatings functionalized with betamethasone on adipose-derived stem cells (ASCs).

    Science.gov (United States)

    Donesz-Sikorska, Anna; Grzesiak, Jakub; Smieszeka, Agnieszk; Krzak, Justyna; Marycz, Krzysztof

    2014-09-01

    Silica-based sol-gel coatings have gained attention in bone therapies and orthopedic applications, due to the biocompatibility and bioactivity, including a high potential for the controlled release both in vitro and in vivo. Bioactive materials are created to facilitate the biocompatibility of orthopedic implants. One of the promising alternatives is biomaterials with immobilized drugs. In this study we demonstrated for the first time novel sol-gel-derived silica coatings with active amino groups (SiO2(NH2)) functionalized with a steroid drug-betamethasone, applied to a substrate 316 L using dip coating technique. The presence of betamethasone in functionalized coatings was directly confirmed by Raman spectroscopy and energy-dispersive X-ray spectroscopic analysis. The wettability was evaluated by the sessile drop method, while the surface free energy was estimated based on the contact angles measured. Our results showed a shift in surface properties from hydrophobic to hydrophilic after application of the coatings. We have investigated the morphology, proliferation factor, and the population doubling time of adipose-derived stem cells for biological purposes. Moreover, the analysis of the distribution and localization of cellular microvesicles was performed to evaluate the influence of functionalized surfaces on cellular cytophysiological activity. Increased proliferation and activation of cells, determined by the observations of microvesicles shedding processes, provided evidence of the availability of the drug. Therefore, we conclude that the sol-gel synthesis proposed here allows to improve the metal substrates and can be successfully used for immobilization of betamethasone. This in turn enables the direct delivery of the drug with implanted material into the wound site, and to stimulate the activity of cells to enhance tissue regeneration.

  1. Preparation of silane-functionalized silica films via two-step dip coating sol-gel and evaluation of their superhydrophobic properties

    Science.gov (United States)

    Ramezani, Maedeh; Vaezi, Mohammad Reza; Kazemzadeh, Asghar

    2014-10-01

    In this paper, we study the two-step dip coating via a sol-gel process to prepare superhydrophobic silica films on the glass substrate. The water repellency of the silica films was controlled by surface silylation method using isooctyltrimethoxysilane (iso-OTMS) as a surface modifying agent. Silica alcosol was synthesized by keeping the molar ratio of ethyltriethoxysilane (ETES) precursor, ethanol (EtOH) solvent, water (H2O) was kept constant at 1:36:6.6 respectively, with 6 M NH4OH throughout the experiment and the percentages of hydrophobic agent in hexane bath was varied from 0 to 15 vol.%. The static water contact angle values of the silica films increased from 108° to 160° with an increase in the vol.% of iso-OTMS. At 15 vol%. of iso-OTMS, the silica film shows static water contact angle as high as 160°. The superhydrophobic silica films are thermally stable up to 440 °C and above this temperature, the silica films lose superhydrophobicity. By controlling the primer particle size of SiO2 about 26 nm, leading to decrease the final size of silica nanoparticles after modification of nanoparticles by isooctyltrimethoxysilane about 42 nm. The films are transparent and have uniform size on the surface. The silica films have been characterized by atomic force microscopy (AFM), fourier transform infrared spectroscopy (FT-IR), transparency, contact angle measurement (CA), Zeta-potential, Thermal stability by TG-DTA analysis.

  2. The use of Liquid Smoke as A Substitute for Nitric Acid for Extraction of Amorphous silica from Rice husk through Sol-Gel Route

    Directory of Open Access Journals (Sweden)

    Wasinton Simanjuntak

    2016-08-01

    Full Text Available This study assessed the potential of liquid smoke as substitute for nitric acid for production of rice husk silica using sol-gel method. The efficacy of liquid smoke was compared to that of 10% HNO3 solution in terms of the volume required and the mass of silica obtained. Further evaluation was made by comparing the characteristics of the silica as revealed by several characterization techniques include Fourier infrared spectroscopy, x-ray diffraction, scanning electron microscopy, and particle size analysis. No significant difference between the volume of the liquid smoke and the HNO3 solution required, as well as between the mass of silica obtained. Both samples display practically similar functionality and structure. The most interesting finding is that the silica obtained using liquid smoke exhibits more homogeneous surface morphology and narrower particle size distribution. Considering its environmentally friendly nature, it was concluded that liquid smoke is more advantageous than HNO3 solution.

  3. Glass powder blended cement hydration modelling

    Science.gov (United States)

    Saeed, Huda

    The use of waste materials in construction is among the most attractive options to consume these materials without affecting the environment. Glass is among these types of potential waste materials. In this research, waste glass in powder form, i.e. glass powder (GP) is examined for potential use in enhancing the characteristics of concrete on the basis that it is a pozzolanic material. The experimental and the theoretical components of the work are carried out primarily to prove that glass powder belongs to the "family" of the pozzolanic materials. The chemical and physical properties of the hydrated activated glass powder and the hydrated glass powder cement on the microstructure level have been studied experimentally and theoretically. The work presented in this thesis consists of two main phases. The first phase contains experimental investigations of the reaction of glass powder with calcium hydroxide (CH) and water. In addition, it includes experiments that are aimed at determining the consumption of water and CH with time. The reactivity, degree of hydration, and nature of the pore solution of the glass powder-blended cement pastes and the effect of adding different ratios of glass powder on cement hydration is also investigated. The experiments proved that glass powder has a pozzolanic effect on cement hydration; hence it enhances the chemical and physical properties of cement paste. Based on the experimental test results, it is recommended to use a glass powder-to-cement ratio (GP/C) of 10% as an optimum ratio to achieve the best hydration and best properties of the paste. Two different chemical formulas for the produced GP C-S-H gel due to the pure GP and GP-CH pozzolanic reaction hydration are proposed. For the pure GP hydration, the produced GP C-S-H gel has a calcium-to-silica ratio (C/S) of 0.164, water-to-silica ratio (H/S) of 1.3 and sodium/silica ratio (N/S) of 0.18. However, for the GP-CH hydration, the produced GP C-S-H gel has a C/S ratio of 1

  4. Research on the properties of SBS modified asphalt with silica hydrated%SBS/白炭黑复配改性沥青性能的研究

    Institute of Scientific and Technical Information of China (English)

    陈淼; 陈浩; 王洪涛; 聂英斌

    2013-01-01

    通过对SBS单一改性沥青和SBS/白炭黑复配改性沥青基本性能的测试,研究了不同改性剂及其掺量对基质沥青性能的影响.结果表明:掺4%SBS改性沥青能够改善基质沥青的高温性能、低温性能和感温性能;掺4%SBS+3%白炭黑复配改性沥青也能改善基质沥青的高温性能、低温性能和感温性能,并且其改善效果优于掺4%SBS单一改性沥青.%In this paper,the properties of SBS modified asphalt with/without silica hydrated were tested,the influence of different modified asphalt and different content of it on the base bitumen were also researched.The results showed that:the hightemperature behavior,low-temperature performance and sensitivity for temperature were improved with 4%SBS content,and the properties can also be improved with 4%SBS and 3% silica hydrated,the latter was better than the former.

  5. Synthesis of organic-inorganic hybrid sols with nano silica particles and organoalkoxysilanes for transparent and high-thermal-resistance coating films using sol-gel reaction.

    Science.gov (United States)

    Na, Moonkyong; Park, Hoyyul; Ahn, Myeongsang; Lee, Hyeonhwa; Chung, Ildoo

    2010-10-01

    Organic-inorganic hybrid sols were synthesized from nano silica particles dispersed in water and from organoalkoxysilanes, using the sol-gel reaction. This work focuses on the effects of the three multifunctional organoalkoxysilanes dimethyldimethoxysilane (DMDMS), methyltrimethoxysilane (MTMS), and tetramethoxysilane (TMOS) to form a transparent and high-thermal-resistance coating film. The stability of the hybrid sol was evaluated as a function of the reaction time for 10 d through the variation of the viscosity. The viscosity of the silica/DMDMS and silica/MTMS sol was slightly increased for 10 d. The multifunctional organoalkoxysilanes formed dense silica networks through hydrolysis and condensation reaction, which enhanced the thermal resistance of the coating films. No thermal degradation of the silica/DMDMS sample occurred up to 600 degrees C, and none of the silica/MTMS and silica/TMOS samples occurred either up to 700 degrees C. The organic-inorganic hybrid sols were coated on the glass substrate using a spin-coating procedure. The organic-inorganic hybrid sols formed flat coating films without cracks. The transmittance of the hybrid sol coating films using MTMS and DMDMS was shown to be over 90%. The transmittance of the silica/TMOS sol coating film reacted for 10 d abruptly decreased due to faster gelation. The silica/DMDMS and silica/MTMS hybrid sols formed smooth coating films while the surface roughness of the silica/TMOS coating film markedly increased when the hybrid sol reacted for 10 d. The increase of the surface roughness of the silica/TMOS coating film can be attributed to the degradation of the stability of the hybrid sol and to the loss of transmittance of the coating film. It was confirmed in this study that the use of organic-inorganic hybrid sol can yield transparent and high-thermal-resistance coating films.

  6. Sol-Gel Synthesis and Luminescent Characteristic of Doped Eu3+ Silicate-Silica Phosphor

    Institute of Scientific and Technical Information of China (English)

    Yang Liangzhun; Yu Xibin; Yang Shiping; Zhou Pingle; Tang Jinfeng; Peng Xiudong

    2005-01-01

    Eu-doped silicate complex gel nano-particles was obtained by sol-gel process and characterized with TEM, XRD, PL, etc. The well dispersed particles have particle size about 60~70 nm with specific surface area 98.3 m2·g-1. The complex gel phosphor gives a broad and strong luminescent emission originating from Eu2+ ions centered at 425 nm. The emission band shifts to shorter wavelengths with the increase of the ion radius of the alkali earth metals, but the band becomes red-shifted gradually with the increase of the ion radius of the alkali metals(except Li+). These divalent Eu2+ ions originate in inequivalent substitution of the alkaline earth ions. The presence of alkaline ions is favorable for the increasing emission intensity of the Eu2+ and lowering crystalline temperature of the silicate complex gel.

  7. Magnetic properties of cobalt ferrite-silica nanocomposites prepared by a sol-gel autocombustion technique

    DEFF Research Database (Denmark)

    Cannas, C.; Musinu, A.; Piccaluga, G.

    2006-01-01

    The magnetic properties of cobalt ferrite-silica nanocomposites with different concentrations (15, 30, and 50 wt %) and sizes (7, 16, and 28 nm) of ferrite particles have been studied by static magnetization measurements and Mossbauer spectroscopy. The results indicate a superparamagnetic behavio...

  8. Effect of Nano-Silica Agglomeration on Hydration and Hardening of Cement%纳米二氧化硅团聚特性对水泥水化硬化性能的影响

    Institute of Scientific and Technical Information of China (English)

    孔德玉; 杜祥飞; 杨杨; Surendra P Shah

    2012-01-01

    Effect of nano-silica agglomeration on the hydration and hardening of cement was investigated by using precipitated silica (PS) with much larger agglomerates and nano-silica (NS) powder with much smaller ones as additives. The results reveal that the PS exhibits a higher pozzolanic reactivity at early ages and a better accelerating effect on the cement hydration though it possesses some larger agglomerates and a little lower pozzolanic reactivity at late ages rather than NS. The observation by scanning electron micros- copy indicates that the cementitious property of the pozzolanic C-S-H gels from the agglomerates was limited. There even existed an interfacial transition zone between the reacted agglomerates and bulk hardened cement paste (HCP). The MIP results show that the NS addition can reduce the capillary and the gel pore of the HCP in the range of 20nm-10 μm more effectively, compared to the PS addition. It is suggested that the effect of nano-silica addition on the microstmcture improvement of the HCP could be resulted fi'om the filling and water adsorbing effects of the agglomerates in the powder rather than the seeding effect.%以团聚粒径很大的沉淀二氧化硅(PS)和团聚粒径较小的纳米二氧化硅(NS)为原材料,研究了纳米二氧化硅团聚特性对水泥水化硬化特性的影响。结果表明:与 NS 相比,虽然 PS 团聚粒径很大,后期火山灰活性较低,其早期火山灰活性却较大,对水泥水化的促进作用也更明显。扫描电子显微镜分析表明,NS 和 PS 的火山灰反应产物的胶结作用有限,其与水泥水化产物本体之间甚至存在明显的界面过渡区。压汞分析表明:掺 PS 和NS 均可有效降低硬化水泥石毛细孔率;与掺 PS 相比,掺 NS 对减小 20 nm~10 μm 的凝胶孔和毛细孔体积更有利。掺纳米二氧化硅对硬化水泥石微观结构的影响主要是由于团聚颗粒对水泥分散体系的填充效应和吸水

  9. Effects of temperature and sodium carboxylate additives on mineralization of calcium oxalate in silica gel systems

    Institute of Scientific and Technical Information of China (English)

    OUYANG; Jianming; DENG; Suiping; LI; Xiangping; TAN; Yanh

    2004-01-01

    calcium oxalate crystals in the presence of membrane vesicles, J. Cryst. Growth, 1993, 134: 211-218.[13]Girija, E. K., Latha, S. C., Kalkura, S. N. et al., Crystallization and microhardness of calcium oxalate monohydrate, Mater. Chem.Phys., 1998, 52: 253-257.[14]Ouyang, J. M., Tan, Y. H., Shen, Y. H., Effect of structurally-specific carboxylate on crystallization of calcium oxalate in gel systems, Acta Physico-Chimca Sinica, 2003, 19(4): 368-371.[15]Ouyang, J. M., Tan, Y. H., Kuang, L. et al., In vitro simulation on the inhibition of calcium oxalate calculus by changing the counterions of citric acid and EDTA, Chin. J. Inorg. Chem. (in Chinese),2003, 19(3): 312-316.[16]Grases, F., Millan, A., Gracia-Raso, A., Polyhydroxycarboxylic acids as inhibitors of calcium oxalate crystal growth; relation between inhibitory capacity and chemical structure, J. Crystal Growth, 1988, 89: 496-500.[17]King, M., McClure, W. F., Andrews, L. C. et al., Powder Diffraction File Alphabetic Index, Inorganic Phases/Organic Phases, International Centre For Diffraction Data, 1601 Park Lane, Pennsylvania, 19081-2389, U.S.A., 1992.[18]Donnet, M., Jongen, N., Lemaitre, J. et al., New morphology of calcium oxalate trihydrate precipitated in a segmented flow tubular reactor, J. Mater. Sci. Lett., 2000, 19: 749-750.[19]Dean, J. A., McGraw-Hill, Lange's Handbook of Chemistry, 13th ed., 1985.[20]Yuzawa, M., Tozuka, K., Tokue, A., Effect of citrate and pyrophosphate on the stability of calcium oxalate dihydrate, Urol. Res.,1998, 26: 83-88.[21]Chernov, A. A., Modern Crystallography Ⅲ, Crystal Growth, Berlin: Springer, 1984, 230.[22]Tomazic, B., Nancollas, G. H., The kinetics of dissolution of calcium oxalate hydrates. Ⅱ. The dihydrate, Invest. Urol., 1980,18(2): 97-101.[23]Tunik, L., Garti, N., Morphological and phase changes in calcium oxalate crystals growth in the presence of sodium diisooctal sulfosuccinate, J. Crystal Growth, 1996, 167: 748-755.[24

  10. Effect of drying on the mesoporous structure of sol-gel derived silica with PPO-PEO-PPO template block copolymer.

    Science.gov (United States)

    Pei, Lihua; Kurumada, Ken-Ichi; Tanigaki, Masataka; Hiro, Masahiko; Susa, Kenzo

    2005-04-01

    The effects of drying method on the pore structure of mesoporous silica were studied from the viewpoint of enhancing closed porosity in mesoporous silica. The mesoporous silica was prepared via a sol-gel process using polyethyleneoxide-polypropyleneoxide-polyethyleneoxide (PEO-PPO-PEO) triblock copolymer (Pluronic P123) as the structure-directing template. The closed porosity was evaluated from the apparent mass density of the sample measured by a helium pycnometer. These mesoporous silicas were also characterized by transmission electron microscopy (TEM), thermogravimetric analysis (TGA), and nitrogen adsorption. The drying method was shown to be responsible for the finally templated mesoporous structure of the silica. More rapid drying is more preferable for enhancing the closed porosity of the mesoporous silica. The closed pores were formed by immediate immobilization of copolymer molecular assemblies in the silica matrix due to the instant removal of the solvent and solidification at higher temperatures. The drying method, mainly affecting the drying rate, is highly influential on the finally replicated mesoporous structure in silica.

  11. Preconcentration of Ni(II on Silica gel Loaded with New Synthesized Schiff base and their Determination by FAAS

    Directory of Open Access Journals (Sweden)

    Hamed Masoudinia

    2014-12-01

    Full Text Available A preconcentration method was developed for the determination of trace amounts of Ni(II by atomic absorption spectrometry. The method is based on the retention of the metal cations by modified silica gel adsorbent. The adsorbed metals were then eluted with nitric acid and the Ni(II was determined by flame atomic absorption spectrometry. The optimal extraction and elution conditions were studied. The effects of diverse ions on the preconcentration were also investigated. A preconcentration factor of 100 can easily be achieved. Calibration graph was obtained and the detection limit of the method for Ni(II was 1.3 ng mL-1. The relative standard deviation (RSD of 0.66–1.32 % was obtained. The method was applied successfully to the determination of Ni(II in water samples.

  12. Efficient and reversible CO2 capture by amine functionalized-silica gel confined task-specific ionic liquid system.

    Science.gov (United States)

    Aboudi, Javad; Vafaeezadeh, Majid

    2015-07-01

    Simple, efficient and practical CO2 capture method is reported using task-specific ionic liquid (IL) supported onto the amine-functionalized silica gel. The results have been shown that both the capacity and rate of the CO2 absorption notably increase in the supported IL/molecular sieve 4 Å system in comparison of homogeneous IL. Additionally, it has shown that the prepared material is capable for reversible carbon dioxide absorption for at least 10 cycles without significant loss of efficiency. The presence of the amine-based IL and the surface bonded amine groups increase the capacity of CO2 absorption even in a CO2/CH4 gas mixture through the formation of ammonium carbamate onto the surface of mesoporous material.

  13. Spectral pH dependence of erythrosin B in sol-gel silica coatings and buffered solutions

    Directory of Open Access Journals (Sweden)

    Montero, E.

    2008-02-01

    Full Text Available Thin coatings optically sensitive against pH are obtained by entrapping erythrosin B molecules in a sol-gel silica matrix. Comparisons between optical spectra of erythrosin B in solutions and those once entrapped in silica coatings are performed for pH ranging from 0.5 to 12.0. Significant differences between both kinds of spectra (solutions and coatings of erythrosin B are observed. Main changes are displayed in the absorption spectra for neutral to basic pH. Furthermore, the erythrosin B doped coatings show memory effect or hysteresis in their spectral response against pH. This means that absorption spectra depend on the direction of the pH change. Likewise, the photoluminescent spectra of erythrosin B in buffered solutions exhibit pH dependence and a maximized response in the basic pH range. On contrast, no significant photoluminescence from the erythrosin B entrapped in the silica coatings is observed. Results are mainly discussed on the basis of different optical response of polyprotic forms of erythrosin B and possible interactions between the molecule and oxygen as well as the porous walls of the sol-gel silica matrix. In addition, the presence of diffusional barriers, which hamper the flowing of protons and other associated ions, is taken into account. Good agreement with previous observations about low absorption of polyprotic cationic and neutral forms of erythrosin B is found.

    Se han obtenido recubrimientos delgados ópticamente sensibles al pH mediante atrapamiento de moléculas de eritrosina B en matrices de sílice obtenidas por sol-gel. Se compara la respuesta espectral de la eritrosina B en solución y atrapada en los recubrimientos de sílice para un intervalo de pH comprendido entre 0,5 y 12. Se observan apreciables diferencias entre ambos tipos de espectros (en solución y en recubrimiento de la eritrosina B. Los principales cambios aparecen en los espectros de absorción para el intervalo neutro y básico de pH. Adem

  14. Efficient and reversible CO2 capture by amine functionalized-silica gel confined task-specific ionic liquid system

    Directory of Open Access Journals (Sweden)

    Javad Aboudi

    2015-07-01

    Full Text Available Simple, efficient and practical CO2 capture method is reported using task-specific ionic liquid (IL supported onto the amine-functionalized silica gel. The results have been shown that both the capacity and rate of the CO2 absorption notably increase in the supported IL/molecular sieve 4 Å system in comparison of homogeneous IL. Additionally, it has shown that the prepared material is capable for reversible carbon dioxide absorption for at least 10 cycles without significant loss of efficiency. The presence of the amine-based IL and the surface bonded amine groups increase the capacity of CO2 absorption even in a CO2/CH4 gas mixture through the formation of ammonium carbamate onto the surface of mesoporous material.

  15. Textural and mechanical characterization of C-S-H gels from hydration of synthetic T1-C3S, β-C2S and their blends

    Directory of Open Access Journals (Sweden)

    Dolado, J. S.

    2011-06-01

    Full Text Available The textural and mechanical characterization of C-S-H gels formed from the hydration of pure T1-C3S, β-C2S and their blends are studied by Nitrogen sorption and nanoindentation experiments. The surface area and nanoporosity of C-S-H gels formed from the hydration of β-C2S and the 30-70 (T1-C3S and β-C2S mixture are higher than those from hydration of T1-C3S, and 70-30, with the difference decreasing with hydration age. Such changes are well supported by findings of nanoindentation study, which shows the greater relative volume of C-S-H phases with lower densities in the β-C2S and the 30-70 pastes. With the increase in hydration age, the relative volume of C-S-H phases with higher densities increased at the expenses of those with lower density. Important quantitative correlations were found among these textural characteristics and the mean chain length, determined from 29Si magic-angle-spinning (MAS NMR, of the C-S-H gels.La caracterización textural y mecánica de geles C-S-H formados a partir de la hidratación de muestras puras de T1-C3S, ß-C2S y sus mezclas ha sido estudiada por medio de adsorción de nitrógeno y nanoindentación. El área superficial y la nano-porosidad de los geles formados durante la hidratación del ß-C2S y la mezcla 30-70 (T1-C3S- ß-C2S son mayores que los correspondientes a los geles del T1-C3S, y la mezcla 70-30; esta diferencia disminuye con el tiempo de hidratación. Estos cambios coinciden con los resultados de nanoindentación que indican un aumento de volumen relativo de las fases C-S-H con una densidad menor en el caso del ß-C2S y la mezcla 30-70. Al aumentar el tiempo de hidratación, el volumen relativo de fases C-S-H de mayor densidad aumenta a expensas de aquellas de menor densidad. Importantes correlaciones cuantitativas se establecen entre las características texturales y la longitud de cadena media del gel C-S-H, determinada mediante RMN-MAS de 29Si.

  16. Adsorption of transition metal ions from aqueous solutions onto a novel silica gel matrix inorganic-organic composite material.

    Science.gov (United States)

    Yin, Ping; Xu, Qiang; Qu, Rongjun; Zhao, Guifang; Sun, Yanzhi

    2010-01-15

    A novel inorganic-organic composite material silica gel microspheres encapsulated by imidazole functionalized polystyrene (SG-PS-azo-IM) has been synthesized and characterized. This composite material was used to investigate the adsorption of Cr(III), Mn(II), Fe(III), Ni(II), Cu(II), Zn(II), Hg(II), Pb(II), Pd(II), Pt(II), Ag(I), and Au(III) from aqueous solutions, and the research results displayed that SG-PS-azo-IM has the highest adsorption capacity for Au(III). Langmuir and Freundlich isotherm models were applied to analyze the experimental data, the best interpretation for the experimental data was given by the Langmuir isotherm equation, and the maximum adsorption capacity for Au(III) is 1.700 mmol/g. The adsorption selectivity, the dynamic adsorption and desorption properties of SG-PS-azo-IM for Au(III) have also been studied. The results showed that SG-PS-azo-IM had excellent adsorption for Au(III) in four binary ions system, especially in the systems of Au(III)-Zn(II) and Au(III)-Cu(II), and almost Au(III) could be desorbed with the eluent solution of 0.5% thiourea in 1 mol/L HCl. Moreover, this novel composite material was used to preconcentrate Au(III) before its determination by flame atomic adsorption spectrometry. In the initial concentration range of 0.10-0.20 microg/mL, multiple of enrichment could reach 5.28. Thus, silica gel encapsulated by polystyrene coupling with imidazole (SG-PS-azo-IM) is favorable and useful for the removal of transition metal ions, and the high adsorption capacity makes it a good promising candidate material for Au(III) removal.

  17. Sorption of the organic cation metoprolol on silica gel from its aqueous solution considering the competition of inorganic cations.

    Science.gov (United States)

    Kutzner, Susann; Schaffer, Mario; Börnick, Hilmar; Licha, Tobias; Worch, Eckhard

    2014-05-01

    Systematic batch experiments with the organic monovalent cation metoprolol as sorbate and the synthetic material silica gel as sorbent were conducted with the aim of characterizing the sorption of organic cations onto charged surfaces. Sorption isotherms for metoprolol (>99% protonated in the tested pH of around 6) in competition with mono- and divalent inorganic cations (Na(+), NH4(+), Ca(2+), and Mg(2+)) were determined in order to assess their influence on cation exchange processes and to identify the role of further sorptive interactions. The obtained sorption isotherms could be described well by an exponential function (Freundlich isotherm model) with consistent exponents (about 0.8). In general, a decreasing sorption of metoprolol with increasing concentrations in inorganic cations was observed. Competing ions of the same valence showed similar effects. A significant sorption affinity of metoprolol with ion type dependent Freundlich coefficients KF,0.77 between 234.42 and 426.58 (L/kg)(0.77) could still be observed even at very high concentrations of competing inorganic cations. Additional column experiments confirm this behavior, which suggests the existence of further relevant interactions beside cation exchange. In subsequent batch experiments, the influence of mixtures with more than one competing ion and the effect of a reduced negative surface charge at a pH below the point of zero charge (pHPZC ≈ 2.5) were also investigated. Finally, the study demonstrates that cation exchange is the most relevant but not the sole mechanism for the sorption of metoprolol on silica gel.

  18. Physical properties of sodium silicate based silica aerogels prepared by single step sol-gel process dried at ambient pressure

    Energy Technology Data Exchange (ETDEWEB)

    Gurav, Jyoti L. [Air Glass Laboratory, Department of Physics, Shivaji University, Kolhapur 416004, Maharashtra (India); Rao, A. Venkateswara [Air Glass Laboratory, Department of Physics, Shivaji University, Kolhapur 416004, Maharashtra (India)], E-mail: raouniv@yahoo.com; Rao, A. Parvathy; Nadargi, D.Y.; Bhagat, S.D. [Air Glass Laboratory, Department of Physics, Shivaji University, Kolhapur 416004, Maharashtra (India)

    2009-05-12

    The experimental results on physical properties of water glass (sodium silicate) based silica aerogels prepared by single step sol-gel process, dried at atmospheric pressure are reported. The hydrolysis and condensation reactions of the sodium silicate precursor proceeded with tartaric acid as a catalyst. The hydrogel was vapour passed in order to remove sodium salt from the gel network. Solvent exchange was carried out using methanol and hexane as a solvents. Finally, surface chemical modification of the gel was done using trimethylchlorosilane (TMCS) followed by ambient pressure drying of the gel up to the temperature 200 deg. C. To get good quality aerogels various sol-gel parameters such as water vapour passing period varied from 0.5 to 2 h, gel aging from 1 to 4 h, Na{sub 2}SiO{sub 3}/H{sub 2}O molar ratio from 3 x 10{sup -3} to 1.5 x 10{sup -2}, tartaric acid/Na{sub 2}SiO{sub 3} molar ratio from 0.3 to 1.9 and TMCS/Na{sub 2}SiO{sub 3} molar ratio from 4.8 to 12. The aerogels were characterized by percentage of volume shrinkage, bulk density, porosity and hydrophobicity. The hydrophobicity of the aerogel was confirmed by Fourier Transform Infrared (FTIR) Spectroscopy and contact angle measurements. Microstructural studies have been carried out by Scanning Electron Microscopy (SEM) and nitrogen adsorption BET analysis. From the TGA-DTA studies of the aerogels, it was found that the aerogels were thermally stable up to 470 {sup o}C. Low density ({approx}0.066 g/cm{sup 3}), high hydrophobicity ({approx}145 deg.), high porosity ({approx}97 %), high pore volume, surface area of 510 m{sup 2}/g aerogels have been obtained for Na{sub 2}SiO{sub 3}:H{sub 2}O:tartaric acid (C{sub 4}H{sub 6}O{sub 6}):TMCS molar ratio at 1:166.6:2.5:12 respectively with half an hour water vapour passing.

  19. [Study on the preparation and properties of novel silica microporous antireflective coating by sol-gel process].

    Science.gov (United States)

    Shang, Meng-Ying; Cao, Lin-Hong; Liu, Miao; Luo, Xuan; Ren, Hong-Bo; Ye, Xin; Tang, Yong-Jian; Jiang, Xiao-Dong

    2013-04-01

    Silica sol was prepared by acid catalyzed sol-gel process using tetraethylorthosilicate (TEOS) as precursor and dimethyldietoxysilane (DDS) as pore-forming agent. A novel kind of monolayer microporous silica anti-reflective (AR) coating was obtained on K9 glass substrate by dip-coating technique and then heat treated at 500 degrees C. The effects of different DDS/TEOS molar ratios on refractive index, transmittance and hardness were investigated. A positive correlation was found between the transmittance and the DDS/TEOS molar ratio due to the increasing porosity. The maximum transmittance can reach 99.7% with the molar ratio of DDS/TEOS rising to 1 : 1. Meanwhile, the refractive index was found quite close to the ideal value 1.22. Nevertheless, higher molar ratio will lead to a bad film-forming property. On the other hand, the hardness of the coatings decreased with the DDS increasing but still remained more than 2 h when the transmittance reached highest. Besides, these coatings exhibit a well abrasion-resistance and excellent adhesivity. The maximum transmittance was only dropped by 0.071% and 0.112% after abrasion for 500 and 1 000 times respectively. Accelerated corrosion tests indicated that the transmittance of traditional coatings rapidly fell down to the substrate level (-92%) after immersion for 5 min, while the transmittance of our novel coating almost linearly decreased and was kept 93.2% after 56 min. In other words, the environment-resistance of our novel silica AR coating is ten times higher than that of traditional ones. The promotions of the coating performances benefit from its micropore structure (-0. 4 nm) with which water molecule can be effectively prevented. With its high transmittance, good mechanical properties and high environment-resistance, this kind of novel coating has a potential application in the field of solar glass modification to improve its anti-reflective properties.

  20. Occlusion of chromophore oxides by Sol-Gel methods: Application to the synthesis of hematite-silica red pigments

    Directory of Open Access Journals (Sweden)

    Vicent, J. B.

    2000-02-01

    Full Text Available Heteromorphic pigments present the chromophore particle occluded in an encapsulating matrix which is thermally stable and insoluble in glazes. The occluded chromophore compound is also insoluble in the host matrix. In this work the mechanisms of formation of this type of pigments are analyzed and the occlusion of hematite into silica matrix is discussed. The formation of this hematite-silica red pigment follows a sintering-coarsening mechanism, and, consequently, the control of both hematite particles nucleation and their crystal growth results to be decisive to obtain a good coloring effectiveness.

    En los pigmentos heteromórficos la partícula de cromóforo es ocluida en una matriz encapsuladora estable tanto termicamente como frente a los vidriados. El compuesto cromóforo ocluido y la matriz no coloreada son insolubles. En este trabajo se analiza los diferentes mecanismos de formación de estos pigmentos heteromórficos y se estudia la oclusión de hematita en sílice mediante métodos sol-gel acuoso. El pigmento sigue un mecanismo de sinterización-crecimiento cristalino por lo que es muy importante controlar el momento de nucleación y la velocidad de crecimiento de las partículas de hematita en el seno de la matriz.

  1. SYNTHESIS OF ZEOLITE SOCONY MOBIL FROM BLUE SILICA GEL AND RICE HUSK ASH AS CATALYSTS FOR HYDROTHERMAL LIQUEFACTION

    Directory of Open Access Journals (Sweden)

    SUYITNO

    2015-08-01

    Full Text Available Renewable biofuels produced by the hydrothermal liquefaction of rice husks have received much attention because of rapid increases in fuel consumption and corresponding declines in fossil fuel resources. To increase biofuel yields, template-free syntheses of Zeolite Socony Mobil (ZSM catalysts based on blue silica gel and rice husk ash as silica sources were studied. After ZSM synthesis in a closed reactor at 170°C, the crystallinity and crystalline diameters of the products were determined by X-ray diffraction, affording values of 56.33%– 65.81% and 64.3–68.5 nm, respectively. The hydrothermal liquefaction of rice husks with or without a catalyst was conducted in a closed reactor (1200 mm length × 100 mm diameter at 275°C for 45 min. The light biofuel was separated from the ethanol solvent and heavy biofuel via vacuum evaporation. The ZSM catalysts increased the biofuel yields by 2.9%–6.0%. The light biofuels exhibited heating values, flash points, and viscosities of approximately 4.2–4.3 kcal·g−1, 19°C, and 1.48–1.52 cSt, respectively. However, further studies are required to enhance the activity of the ZSMs and increase the quality of the biofuels.

  2. Trivalent chromium removal from aqueous solutions by a sol–gel synthesized silica adsorbent functionalized with sulphonic acid groups

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Gonzalez, Sergio Efrain [Departamento de Ingeniería Química, Universidad de Guadalajara, Blvd. Marcelino García Barragán # 1421, esq. Calzada Olímpica, C.P. 44430 Guadalajara, Jalisco (Mexico); Carbajal-Arizaga, Gregorio Guadalupe [Departamento de Química, CUCEI, Universidad de Guadalajara, Blvd. Marcelino García Barragán # 1421, esq. Calzada Olímpica, C.P. 44430 Guadalajara, Jalisco (Mexico); Manriquez-Gonzalez, Ricardo [Departamento de Madera, Celulosa y Papel, CUCEI, Universidad de Guadalajara, Km 15.5, carretera Guadalajara-Nogales, Las Agujas, C.P. 45020 Zapopan, Jalisco (Mexico); De la Cruz-Hernandez, Wencel [Centro de Nanociencias y Nanotecnología, Universidad Nacional Autónoma de México, Km 107 carretera Tijuana-Ensenada, C.P. 22830 Ensenada, Baja California (Mexico); Gomez-Salazar, Sergio, E-mail: sergio.gomez@cucei.udg.mx [Departamento de Ingeniería Química, Universidad de Guadalajara, Blvd. Marcelino García Barragán # 1421, esq. Calzada Olímpica, C.P. 44430 Guadalajara, Jalisco (Mexico)

    2014-11-15

    Highlights: • Corpuscular sulphonic acid-functionalized silica holds improved uptake of chromium. • Mesopores on adsorbent facilitate (CH{sub 3}COO){sub 2}Cr{sup +} ion uptake on sulphonate sites. • Formation of chromium acetate sulphonate complex proposed from XPS results. • Fixed bed chromium uptake results suggest potential industrial use. - Abstract: A high capacity hybrid silica adsorbent was synthesized via sol–gel processing with sulphonic acid groups as trivalent chromium complex ions chelators from aqueous solutions. The synthesis included co-condensation of tetraethoxysilane (TEOS) with 3-(mercaptopropyl)trimethoxysilane (MPS), and oxidation of thiol to sulphonic acid groups. Chromium uptake kinetic, batch and fixed-bed experiments were performed to assess the removal of this metal from aqueous solutions. {sup 13}C, {sup 29}Si CPMAS NMR, FTIR, XPS were used to characterize the adsorbent structure and the nature of chromium complexes on the adsorbent surface. Chromium maximum uptake was obtained at pH 3 (72.8 mg/g). Elemental analysis results showed ligand density of 1.48 mmol sulphonic groups/g. About 407 mL of Cr(III) solution (311 mg/L) were treated to breakthrough point reaching ≤0.06 mg/L at the effluent. These results comply with USEPA regulation for chromium concentration in drinking water (≤0.1 mg/L). The adsorbent shows potential to be used in chromium separations to the industrial level.

  3. Preparation and characterization of EPDM/silica composites prepared through non-hydrolytic sol-gel method in the absence and presence of a coupling agent

    Directory of Open Access Journals (Sweden)

    T. H. Mokhothu

    2014-11-01

    Full Text Available Ethylene propylene diene monomer (EPDM rubber composites containing in situ generated silica particles was prepared through a non-hydrolytic sol-gel (NHSG method with silicon tetrachloride as precursor. The silica particles were homogenously dispersed in the EPDM matrix, but there were agglomerates at high silica contents. The swelling experiments showed a decrease in the crosslinking density of the vulcanized rubber due to the presence of the silica particles for both the composites prepared in the presence and absence of a coupling agent, bis-[-3-(triethoxysilyl-propyl]-tetrasulfide (TESPT. Unlike the composites prepared through a hydrolytic sol-gel (HSG method with TEOS as precursor, the TESPT did not seem to take part in the sol-gel reaction. The presence of TESPT influenced the interaction and dispersion of the silica particles in the EPDM matrix, which gave rise to increased thermal stability of the EPDM when compared to the composites prepared in the absence of TESPT. However, ethylene chloride and TESPT evaporated from the samples at temperatures below the EPDM decomposition range. The values of the Nielsen model parameters, that gave rise to a good agreement with the experimentally determined Young’s modulus values, indicated improved dispersion and reduced size of the silica aggregates in the EPDM matrix. There was also good agreement between the storage modulus and Young’s modulus values. The filler effectiveness (Factor C indicated a mechanical stiffening effect and a thermal stability contribution by the filler, while the damping reduction (DR values confirmed that the EPDM interacted strongly with the well dispersed silica particles and the polymer chain mobility was restricted. The tensile properties, however, were in some cases worse than those for the samples prepared through the HSG method in the presence of TEOS.

  4. The influence of the hydrophobic agent, catalyst, solvent and water content on the wetting properties of the silica films prepared by one-step sol–gel method

    Energy Technology Data Exchange (ETDEWEB)

    Ramezani, Maedeh, E-mail: m.ramezani@merc.ac.ir [Division of Nanotechnology and Advanced Materials, Materials and Energy Research Center, P.O. Box 31787-316, Karaj (Iran, Islamic Republic of); Vaezi, Mohammad Reza [Division of Nanotechnology and Advanced Materials, Materials and Energy Research Center, P.O. Box 31787-316, Karaj (Iran, Islamic Republic of); Kazemzadeh, Asghar [Division of Semiconductors, Materials and Energy Research Center, P.O. Box 31787-316, Karaj (Iran, Islamic Republic of)

    2015-01-30

    Graphical abstract: - Highlights: • Transparent, hydrophobic, uniform silica film by sol–gel co-precursor process. • Preparation of silica coatings from ETES and Iso-OTMS in different molar ratios. • Decreasing in hydrophobicity of the films with increasing in Iso-TMS molar ratio. • By changing the molar ratio of component, different size of particles was obtained. - Abstract: In this paper, we used one-step sol–gel process to prepare the hydrophobic silica films on the glass substrate from the ethyltriethoxysilane (ETES) as a precursor and iso-octyltrimethoxysilane (Iso-OTMS) as a hydrophobic agent. In order to study the effect of the hydrophobic agent on the water repellent properties of the silica films, the alcosol was prepared by keeping constant the molar ratio of ETES:EtOH:H{sub 2}O at 1:36.2:6.3, with 6 M ammonium hydroxide and Iso-OTMS/ETES molar ratio varied from 0.2 to 1.4. Also, we investigated the influence of the other sol–gel reaction parameters, such as catalyst, solvent and water content and their effect on the morphology and hydrophobic properties of the silica films. The results revealed that by altering the molar ratio of NH{sub 4}OH, EtOH and H{sub 2}O, different sizes of silica nanoparticles from 41.24 to 86.16 nm were obtained. The silica films were characterized by atomic force microscopy (AFM), Fourier transform infrared spectroscopy (FT-IR), field emission scanning electron microscopy (FE-SEM) images, contact angle measurement (CA) and percentage of optical transmission.

  5. Application of microwave-assisted desorption/headspace solid-phase microextraction as pretreatment step in the gas chromatographic determination of 1-naphthylamine in silica gel adsorbent.

    Science.gov (United States)

    Yan, Cheing-Tong; Jen, Jen-Fon; Shih, Tung-Sheng

    2007-03-30

    Pretreatment of silica gel sample containing 1-naphthylamine by microwave-assisted desorption (MAD) coupled to in situ headspace solid phase microextraction (HS-SPME) has been investigated as a possible alternative to conventional methods prior to gas chromatographic (GC) analysis. The 1-naphthylamine desorbs from silica gel to headspace under microwave irradiation, and directly absorbs onto a SPME fiber located in a controlled-temperature headspace area. After being collected on the SPME fiber, and desorbed in the GC injection port, 1-naphthylamine is analyzed by GC-FID. Parameters that influence the extraction efficiency of the MAD/HS-SPME, such as the extraction media and its pH, the microwave irradiation power and irradiation time as well as desorption conditions of the GC injector, have been investigated. Experimental results indicate that the extraction of a 150mg silica gel sample by using 0.8ml of 1.0M NaOH solution and a PDMS/DVB fiber under high-powered irradiation (477W) for 5min maximizes the extraction efficiency. Desorption of 1-naphthylamine from the SPME fiber in GC injector is optimal at 250 degrees C held for 3min. The detection limit of method is 8.30ng. The detected quantity of 1-naphthylamine obtained by the proposed method is 33.3 times of that obtained by the conventional solvent extraction method for the silica gel sample containing 100ng of 1-naphthylamine. It provides a simple, fast, sensitive and organic-solvent-free pretreatment procedure prior to the analysis of 1-naphthylamine collected on a silica gel adsorbent.

  6. Synthesis and characterization of polymer-silica hybrid latexes and sol-gel-derived films

    Science.gov (United States)

    Petcu, Cristian; Purcar, Violeta; Ianchiş, Raluca; Spătaru, Cătălin-Ilie; Ghiurea, Marius; Nicolae, Cristian Andi; Stroescu, Hermine; Atanase, Leonard-Ionuţ; Frone, Adriana Nicoleta; Trică, Bogdan; Donescu, Dan

    2016-12-01

    Sol-gel derived organic-inorganic hybrid systems were obtained by applying alkaline-catalyzed co-hydrolysis and copolycondensation reactions of tetraethoxysilane (TEOS), methyltriethoxysilane (MTES), isobutyltriethoxysilane (IBTES), diethoxydimethylsilane (DMDES), and vinyltriethoxysilane (VTES), respectively, into a polymer latex functionalized with vinyltriethoxysilane (VTES). The properties of the latex hybrid materials were analyzed by FTIR, water contact angle, environmental scanning electron microscopy (ESEM), TEM and AFM analysis, respectively. FT-IR spectra confirmed that the chemical structures of the sol-gel derived organic-inorganic materials are changed as function of inorganic precursor and Sisbnd Osbnd Si networks are formed during the co-hydrolysis and copolycondensation reactions. The water contact angle on the sol-gel latex film containing TEOS + VTES increased to 135° ± 2 compared to 65° ± 5 for the blank latex, due VTES incorporation into latex material. TGA curves of hybrid sample modifies against neat polymer, the thermal stability being influenced by the presence of the inorganic partner. ESEM analysis showed that the latex hybrid films prepared with different inorganic precursors were formed and the Si-based polymers were distributed on the surface of the dried sol-gel hybrid films. TEM and AFM photos revealed that the latex emulsion morphology was modified due to the VTES incorporation into system.

  7. Sol–gel-based silver nanoparticles-doped silica – Polydiphenylamine nanocomposite for micro-solid-phase extraction

    Energy Technology Data Exchange (ETDEWEB)

    Bagheri, Habib, E-mail: bagheri@sharif.edu; Banihashemi, Solmaz

    2015-07-30

    A nanocomposite of silica-polydiphenylamine doped with silver nanoparticles (Ag–SiO{sub 2}-PDPA) was successfully synthesized by the sol–gel process. For its preparation, PDPA was mixed with butanethiol capped Ag nanoparticles (NPs) and added to the silica sol solution. The Ag NPs were stabilized as a result of their adsorption on the SiO{sub 2} spheres. The surface characteristic of nanocomposite was investigated using scanning electron microscopy (SEM). In this work the Ag–SiO{sub 2}-PDPA nanocomposite was employed as an efficient sorbent for micro-solid-phase extraction (μ-SPE) of some selected pesticides. An amount of 15 mg of the prepared sorbent was used to extract and determine the representatives from organophosphorous, organochlorine and aryloxyphenoxy propionic acids from aqueous samples. After the implementation of extraction process, the analytes were desorbed by methanol and determined using gas chromatography–mass spectrometry (GC–MS). Important parameters influencing the extraction and desorption processes such as pH of sample solution, salting out effect, type and volume of the desorption solvent, the sample loading and eluting flow rates along with the sample volume were experimentally optimized. Limits of detection (LODs) and the limits of quantification (LOQs) were in the range of 0.02–0.05 μg L{sup −1} and 0.1–0.2 μg L{sup −1}, respectively, using time scheduled selected ion monitoring (SIM) mode. The relative standard deviation percent (RSD %) with four replicates was in the range of 6–10%. The applicability of the developed method was examined by analyzing different environmental water samples and the relative recovery (RR %) values for the spiked water samples were found to be in the range of 86–103%. - Highlights: • A sol–gel-based silver nanoparticles doped silica-polydiphenylamine nanocomposite was synthesized. • The sorbent was applied to micro-solid-phase extraction of some selected pesticides in water

  8. A new separation and preconcentration method for selenium in some foods using modified silica gel with 2,6-diamino-4-phenil-1,3,5-triazine.

    Science.gov (United States)

    Mendil, Durali; Demirci, Zafer; Uluozlu, Ozgur Dogan; Tuzen, Mustafa; Soylak, Mustafa

    2017-04-15

    A novel and simple solid phase extraction method was improved and recommended for selenium. Silica gel was modified with 2,6-diamino-4-phenil-1,3,5-triazine and characterized by FTIR, SEM and elemental analysis and used adsorbent for column solid phase extraction of selenium ions. The experimental parameters (pH, flow rates, amounts of the modified silica gel, concentration and type of eluent, volume of sample, etc.) on the recoveries of selenium were optimized. Standard reference materials were analyzed for validation of method. The present method was successfully applied to the detection of total selenium in water and microwave digested some food samples with quantitative recoveries (> 95%). The relative standard deviations weresilica gel was 5.90mgg(-1). The LOD was 0.015μgL(-1). Enrichment factor was obtained as 50 for the introduced method.

  9. Phenyl Functionalized Sol-gel Silica Sorbent for Capillary Microextraction and Chromia-Based Sol-gel Ucon Stationary Phase for Capillary Gas Chromatography

    Science.gov (United States)

    McLean, Michael M.

    The first chapter of this thesis presents an introduction to sol-gel methodology whose usefulness as a synthetic route will be demonstrated with two applications in chromatography. The first application involves the fabrication of a capillary micro-extraction (CME) device by coating a phenyl functionalized extracting phase on the inner surface of a fused silica capillary for analyte pre-concentration. The device was coupled on-line to a RP-HPLC system and practicality was demonstrated using allergens as target analytes. The allergens chosen as model analytes are typically found in fragrance products and food. Most of the 26 fragrance allergens that are monitored by various government authorities have a phenyl organic moiety (a strong chromophore), thus making them appropriate probes for exploring the extraction efficiency of the coating using a UV detector. The CME device showed ppt level limit of detection which makes it suitable for trace analyses of allergens and similar compounds in a variety of matrices. The second application explores the feasibility of using sol-gel derived chromia-based stationary phase in gas chromatographic columns. The organic moiety of the stationary phase was derived from Ucon 75-H-90,000 while the inorganic backbone was prepared using chromium(III) dichloride hydroxide - methacrylic acid - aqua complex, 40% in isopropanol/acetone . Usefulness of prepared chromia-based GC stationary phase was examined for petrochemical application. Promising results were obtained using aliphatic-aromatics, polyaromatic hydrocarbons, BTEX test mixture, cycloalkanes, branched alkanes and akylbenzenes. The column was able to perform without degradation despite being rinsed multiples times sequentially with the following solvents: dichloromethane, methanol, water and finally methanol again. Maximum theoretical plate number calculated is around 2,400 plates/m. The plate number clearly needs improvement but is a promising result for the newly explored

  10. Silica/polyacrylonitrile hybrid nanofiber membrane separators via sol-gel and electrospinning techniques for lithium-ion batteries

    Science.gov (United States)

    Yanilmaz, Meltem; Lu, Yao; Zhu, Jiadeng; Zhang, Xiangwu

    2016-05-01

    Silica/polyacrylonitrile (SiO2/PAN) hybrid nanofiber membranes were fabricated by using sol-gel and electrospinning techniques and their electrochemical performance was evaluated for use as separators in lithium-ion batteries. The aim of this study was to design high-performance separator membranes with enhanced electrochemical performance and good thermal stability compared to microporous polyolefin membranes. In this study, SiO2 nanoparticle content up to 27 wt% was achieved in the membranes by using sol-gel technique. It was found that SiO2/PAN hybrid nanofiber membranes had superior electrochemical performance with good thermal stability due to their high SiO2 content and large porosity. Compared with commercial microporous polyolefin membranes, SiO2/PAN hybrid nanofiber membranes had larger liquid electrolyte uptake, higher electrochemical oxidation limit, and lower interfacial resistance with lithium. SiO2/PAN hybrid nanofiber membranes with different SiO2 contents (0, 16, 19 and 27 wt%) were also assembled into lithium/lithium iron phosphate cells, and high cell capacities and good cycling performance were demonstrated at room temperature. In addition, cells using SiO2/PAN hybrid nanofiber membranes with high SiO2 contents showed superior C-rate performance compared to those with low SiO2 contents and commercial microporous polyolefin membrane.

  11. Sol-gel synthesis of iron catalysers supported on silica and titanium for selectively oxidising methane to formaldehyde

    Directory of Open Access Journals (Sweden)

    Carlos Alberto Guerrero Fajardo

    2010-07-01

    Full Text Available Iron materials supported on silica were prepared by the sol-gel method for evaluating catalytic activity in selective o-xidation of methane to formaldehyde. Four catalysts were prepared, one corresponding to the silica support (catalyst 1S, another to the titanium support (catalyst 1T and two more having 0.5% weight iron loads, one for the silica su-pport (catalyst 2FS and the last one the titanium support (catalyst 2FT. The higher BET areas were 659 and 850 m2/g for catalysts 1S and 2FS, respectively while catalysts 1T and 2FT displayed areas of 65 and 54 m2/g, respec-tively. Scanning and transmission electronic microscopy displayed an amorphous structure in the silica-supported materials while titanium-supported materials displayed dense materials having defined structure. X-ray diffraction confirmed the silica’s amorphous structure in 1S and 2FS catalysts and displayed the 1T and 2FT catalysts’ anatase structure. The programmed temperature reduction for the 1S and 2FS catalysts did not display reducible species, while displaying hydrogen consumption peaks related to Fe3O4 reduction to α-Fe via FexO route for 1T and 2FT ca-talysts. The electronic spectroscopy X-ray photo confirmed the Fe(III specie as having 710.6 e.V binding energy for both 2FS and 2FT catalysts. Catalytic activity was carried out at atmospheric pressure in a quartz reactor, reaction mixture as CH4/O2/N2 =7.5/1/4 at 400-800°C temperature range. The reaction products were analysed by gas chromatography on Hayesep R and T columns using 5Å molecular screening. The best response for selective oxida-tion of methane to formaldehyde was displayed by the 2FS catalyst with 3.4% mol methane conversion at 650°C, 11.9% mol formaldehyde selectivity and 0.0211 g HCHO/Kg catalyst yield.

  12. Selective Pre-concentration and Solid Phase Extraction of Mercury(Ⅱ) from Natural Water by Silica Gel-loaded(E)-N-(1-Thien-2'-ylethylidene)-1,2-phenylenediamine Phase

    Institute of Scientific and Technical Information of China (English)

    MOGHIMI Ali

    2007-01-01

    Silica gel-loaded (E)-N-(1-thien-2'-ylethylidene)-1,2-phenylenediamine (TEPDA) phase was synthesized based on physical adsorption approaches. The stability of a chemically modified TEPDA especially in concentrated hydrochloric acid that was then used as a recycling and preconcentration reagent allowed the further uses of silica gel-loadej immobilized TEPDA phase. The application of this silica gel-loaded phase to sorption of a series of metal ions was performed by using different controlling factors such as the pH of the metal ion solution and the equilibration shaking time by the static technique. This difference was interpreted on the basis of selectivity incorporated in these sulfur containing silica gel-loaded TEPDA phases. Hg(Ⅱ) was found to exhibit the highest affinity towards extraction by these silica gel-loaded TEPDA phases. The pronounced selectivity was also confirmed by the determined distribution coefficients (Kd) of all the metal ions, showing the highest value reported for mercury(Ⅱ)extraction by the silica gel immobilized TEPDA phase. The potential applications of the silica gel immobilized TEPDA phase to selective extraction of mercury(Ⅱ) from aqueous solution were successfully accomplished and preconcentration of low concentration of Hg(Ⅱ) (30 pg·mL-1) from natural tap water with a preconcentration factor of 200 for Hg(Ⅱ) off-line analysis was conducted by cold vapor atomic absorption analysis.

  13. Enhancement of proteolysis through the silica-gel-derived microfluidic reactor.

    Science.gov (United States)

    Liu, Yun; Qu, Haiyun; Xue, Yan; Wu, Zhonglin; Yang, Pengyuan; Liu, Baohong

    2007-05-01

    An on-chip enzymatic reactor providing rapid protein digestion is presented. Trypsin-embedding stationary phase within the microchannel has been prepared by the sol-gel method. Such a microfluidic reactor has been used for low-level protein digestion at 16 fmol per analysis. The analytical potential of the microreactor combined with the strong cation exchange and RPLC ESI-MS/MS for the identification of real samples from the cytoplasma of the human liver tissue has been demonstrated.

  14. Growth and characterization of cerium lanthanum oxalate crystals grown in hydro-silica gel

    Energy Technology Data Exchange (ETDEWEB)

    John, M.V.; Ittyachen, M.A. [Mahatma Gandhi Univ., Kerala (India). School of Pure and Applied Physics

    2001-07-01

    Single crystals of mixed cerium lanthanum oxalate (CLO) are grown by gel method. Over the hydrosilica gel prepared by mixing oxalic acid and sodium meta silicate, a mixture of aqueous solutions of cerium nitrate and lanthanum nitrate are poured gently. Cerium and lanthanum ions diffuse into the gel and react with oxalic acid to give colorless, transparent cerium lanthanum oxalate crystals with in a few days. Different growth parameters give crystals of various dimensions. Infrared (IR) spectrum confirms the presence of water molecules and carboxylic acid. X-ray diffraction (XRD) pattern of these samples reveals the crystalline nature. Diffraction peaks are indexed. Unit cell parameters are determined. Thermogravimetric analysis (TGA) and differential thermal analysis (DTA) data support the presence of 9 H{sub 2}O molecules attached to the CLO crystal lattice which are lost around 200 C as revealed by the endotherm record. Exothermic peak around 350 C-425 C shows the release of CO and CO{sub 2}. Elemental analysis done by energy dispersive X-ray fluorescence analysis (EDXRF) for the mixed rare earth compound is almost in good agreement with experimental and theoretical values. (orig.)

  15. Effects of a Protic Ionic Liquid on the Reaction Pathway during Non-Aqueous Sol–Gel Synthesis of Silica: A Raman Spectroscopic Investigation

    Directory of Open Access Journals (Sweden)

    Anna Martinelli

    2014-04-01

    Full Text Available The reaction pathway during the formation of silica via a two-component “non-aqueou” sol-gel synthesis is studied by in situ time-resolved Raman spectroscopy. This synthetic route is followed with and without the addition of the protic ionic liquid 1-ethylimidazolium bis(trifluoromethanesulfonylimide (C2HImTFSI in order to investigate its effect on the reaction pathway. We demonstrate that Raman spectroscopy is suitable to discriminate between different silica intermediates, which are produced and consumed at different rates with respect to the point of gelation. We find that half-way to gelation monomers and shorter chains are the most abundant silica species, while the formation of silica rings strongly correlates to the sol-to-gel transition. Thus, curling up of linear chains is here proposed as a plausible mechanism for the formation of small rings. These in turn act as nucleation sites for the condensation of larger rings and thus the formation of the open and polymeric silica network. We find that the protic ionic liquid does not change the reaction pathway per se, but accelerates the cyclization process, intermediated by the faster inclusion of monomeric species.

  16. Preparation of glucose oxidase electrode containing hydrophobic silica nanoparticles by the sol-gel method

    Institute of Scientific and Technical Information of China (English)

    张琳; 唐芳琼; 袁金锁; 江龙

    1995-01-01

    The influences of hydrophobic SiO2 nanoparticles and the contents of glucose oxidase(GOD)upon the response current of enzyme electrode have been investigated by using the sol-gel method,in whichpolyvinylbutyryl(PVB)was used as a matrix.The influenoe of enzymatic activity was measured byelectrochemical method.Experimental data demonstrated that hydrophobic SiO2 particles can immobilizeenzyme well,providing a good and simple method for preparing high quality GOD biosensor.The mechanismhas been discussed.

  17. Three Gel States of Colloidal Composites Consisting of Polymer-Brush-Afforded Silica Particles and a Nematic Liquid Crystal with Distinct Viscoelastic and Optical Properties.

    Science.gov (United States)

    Kawata, Yuki; Yamamoto, Takahiro; Kihara, Hideyuki; Yamamura, Yasuhisa; Saito, Kazuya; Ohno, Kohji

    2016-11-02

    Colloidal composites consisting of polymer-brush-afforded silica particles (P-SiPs) and a nematic liquid crystal (LC) exhibited three gel states with distinct viscoelastic and/or optical properties depending on temperature: (1) opaque hard gel, (2) translucent hard gel, and (3) translucent soft gel. We demonstrated that the transitions of the optical property and the hardness of the gels were due to the phase transition of the LC matrix and the glass transition of the grafted polymers of P-SiPs, respectively. We then revealed that the gelation (the formation of the translucent soft gel) was caused by the phase separation of P-SiPs and LC matrix in an isotropic phase based on spinodal decomposition. In addition, the particle concentration and molecular weight of the grafted polymer of P-SiPs were observed to significantly affect the elastic moduli and thermal stability of the composite gels. By the addition of an azobenzene derivative into an LC matrix, we achieved photochemical switching of the transparency of the composites based on the photoinduced phase transition of LCs, while keeping self-supporting ability of the composite gel.

  18. Construction and evaluation of As(V) selective electrodes based on iron oxyhydroxide embedded in silica gel membrane

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez, J.A. [Departamento de Quimica Analitica, Facultad de Ciencias, Universidad de Valladolid, Prado de la Magdalena s/n, 47005 Valladolid (Spain); Centro de Investigaciones Quimicas, Universidad Autonoma del Estado de Hidalgo, Crta. Pachuca-Tulancingo, Km 4.5, 42076 Pachuca, Hidalgo (Mexico); Barrado, E. [Departamento de Quimica Analitica, Facultad de Ciencias, Universidad de Valladolid, Prado de la Magdalena s/n, 47005 Valladolid (Spain)]. E-mail: ebarrado@qa.uva.es; Vega, M. [Departamento de Quimica Analitica, Facultad de Ciencias, Universidad de Valladolid, Prado de la Magdalena s/n, 47005 Valladolid (Spain); Prieto, F. [Centro de Investigaciones Quimicas, Universidad Autonoma del Estado de Hidalgo, Crta. Pachuca-Tulancingo, Km 4.5, 42076 Pachuca, Hidalgo (Mexico); Lima, J.L.F.C. [REQUIMTE/Departamento de Quimica-Fisica, Faculdade de Farmacia, Universidade do Porto, Rua Anibal Cunha, 164, 4099-030 Porto (Portugal)

    2005-05-10

    Two As(V) selective electrodes (with and without inner reference solution) have been developed using selective membranes based on iron oxyhydroxide embedded on silica gel mixed with ultrapure graphite at a 2/98 (w/w) ratio. The active component of the membrane was synthesised by means of the sol-gel technique and characterized by X-ray and FTIR spectroscopy. This compound shows a great affinity towards As(V) ions adsorbing 408 mg g{sup -1}. Using 1 mol l{sup -1} phosphate buffer (at a 1/1, v/v ratio) to adjust the pH and the ionic strength to 7 and 0.5 mol l{sup -1}, respectively, the calibration curve is linear from 1.0 x 10{sup -1} to 1.0 x 10{sup -6} mol l{sup -1} As(V), with a practical detection limit of 4 x 10{sup -7} mol l{sup -1} (0.03 mg l{sup -1}) and a slope close to 30 mV decade{sup -1}. The effect of potentially interfering ions was investigated. The accuracy and precision of the procedure have been tested on arsenic-free drinking water samples spiked with known amounts of arsenic and on groundwater samples containing high levels of arsenic. Total arsenic in these samples was determined after oxidation of As(III) with iodine at pH 7. The results of total As were comparable to those generated by ET-AAS.

  19. Silica-polyethylene glycol hybrids synthesized by sol-gel: Biocompatibility improvement of titanium implants by coating.

    Science.gov (United States)

    Catauro, M; Bollino, F; Papale, F; Ferrara, C; Mustarelli, P

    2015-10-01

    Although metallic implants are the most used in dental and orthopaedic fields, they can early fail due to low tissue tolerance or osseointegration ability. To overcome this drawback, functional coatings can be applied on the metallic surface to provide a firm fixation of the implants. The objective of the present study was twofold: to synthesize and to characterize silica/polyethylene glycol (PEG) hybrid materials using sol-gel technique and to investigate their capability to dip-coat titanium grade 4 (Ti-gr4) substrates to improve their biological properties. Various hybrid systems have been synthesized by changing the ratio between the organic and inorganic phases in order to study the influence of the polymer amount on the structure and, thus, on the properties of the coatings. Fourier transform infrared (FTIR) spectroscopy and solid state Nuclear Magnetic Resonance (NMR) allowed us to detect the formation of hydrogen bonds between the inorganic sol-gel matrix and the organic component. SEM analysis showed that high PEG content enables to obtain crack free-coating. Moreover, the effective improvement in biological properties of Ti-gr4 implants has been evaluated by performing in vitro tests. The bioactivity of the hybrid coatings has been showed by the hydroxyapatite formation on the surface of SiO2/PEG coated Ti-gr4 substrates after soaking in a simulated body fluid and the lack of cytotoxicity by the WST-8 Assay. The results showed that the coated substrates are more bioactive and biocompatible than the uncoated ones and that the bioactivity is not significantly affected by PEG amount whereas its addition makes the films more biocompatible.

  20. Erbium-activated silica-zirconia planar waveguides prepared by sol-gel route

    Energy Technology Data Exchange (ETDEWEB)

    Goncalves, Rogeria R. [Departamento de Quimica, Faculdade de Filosofia, Ciencias e Letras de Ribeirao Preto, Universidade de Sao Paulo-Av., Bandeirantes 3900, cep 14040-901, Ribeirao Preto-SP (Brazil)], E-mail: rrgoncalves@ffclrp.usp.br; Messaddeq, Younes [Instituto de Quimica, UNESP-Rua Prof. Francisco Degni, s/n, Quitandinha, cep 14800-900 Araraquara-SP (Brazil); Chiasera, Alessandro; Jestin, Yoann; Ferrari, Maurizio [CNR-IFN, Istituto di Fotonica e Nanotecnologie, CSMFO group, via Sommarive 14, 38050 Povo, Trento (Italy); Ribeiro, Sidney J.L. [Instituto de Quimica, UNESP-Rua Prof. Francisco Degni, s/n, Quitandinha, cep 14800-900 Araraquara-SP (Brazil)

    2008-03-31

    Er{sup 3+} doped (100 - x)SiO{sub 2} - xZrO{sub 2} planar waveguides were prepared by the sol-gel route, with x ranging from 10 up to 30 mol%. Multilayer films doped with 0.3 mol% Er{sup 3+} ions were deposited on fused quartz substrates by the dip-coating technique. The thickness and refractive index were measured by m-line spectroscopy at different wavelengths. The fabrication protocol was optimized in order to confine one propagating mode at 1.5 {mu}m. Photoluminescence in the near and visible region indicated a crystalline local environment for the Er{sup 3+} ion.

  1. Characterization of pure and copper-doped iron tartrate crystals grown in silica gel

    Indian Academy of Sciences (India)

    V Mathivanan; M Haris

    2013-07-01

    Single crystal growth of pure and copper-doped iron tartrate crystals bearing composition Cu Fe(1−) C4H4O6 · H2O, where = 0, 0.07, 0.06, 0.05, 0.04, 0.03, is achieved using gel technique. The elemental analysis has been done using energy-dispersive X-ray analysis (EDAX) spectrum. The characterization studies such as Fourier transform infrared spectroscopy (FTIR), powder X-ray diffraction (XRD), magnetic analysis and thermal analysis have been done for crystals with = 0 for pure iron tartrate and with = 0.05 for copper-mixed iron tartrate crystals. A detailed comparison has been made between pure and doped crystals.

  2. Magnetic properties of cobalt ferrite-silica nanocomposites prepared by a sol-gel autocombustion technique.

    Science.gov (United States)

    Cannas, C; Musinu, A; Piccaluga, G; Fiorani, D; Peddis, D; Rasmussen, H K; Mørup, S

    2006-10-28

    The magnetic properties of cobalt ferrite-silica nanocomposites with different concentrations (15, 30, and 50 wt %) and sizes (7, 16, and 28 nm) of ferrite particles have been studied by static magnetization measurements and Mossbauer spectroscopy. The results indicate a superparamagnetic behavior of the nanoparticles, with weak interactions slightly increasing with the cobalt ferrite content and with the particle size. From high-field Mossbauer spectra at low temperatures, the cationic distribution and the degree of spin canting have been estimated and both parameters are only slightly dependent on the particle size. The magnetic anisotropy constant increases with decreasing particle size, but in contrast to many other systems, the cobalt ferrite nanoparticles are found to have an anisotropy constant that is smaller than the bulk value. This can be explained by the distribution of the cations. The weak dependence of spin canting degree on particle size indicates that the spin canting is not simply a surface phenomenon but also occurs in the interiors of the particles.

  3. Development of a bi-functional silica monolith for electro-osmotic pumping and DNA clean-up/extraction using gel-supported reagents in a microfluidic device.

    Science.gov (United States)

    Oakley, Jennifer A; Shaw, Kirsty J; Docker, Peter T; Dyer, Charlotte E; Greenman, John; Greenway, Gillian M; Haswell, Stephen J

    2009-06-07

    A silica monolith used to support both electro-osmotic pumping (EOP) and the extraction/elution of DNA coupled with gel-supported reagents is described. The benefits of the combined EOP extraction/elution system were illustrated by combining DNA extraction and gene amplification using the polymerase chain reaction (PCR) process. All the reagents necessary for both processes were supported within pre-loaded gels that allow the reagents to be stored at 4 degrees C for up to four weeks in the microfluidic device. When carrying out an analysis the crude sample only needed to be hydrodynamically introduced into the device which was connected to an external computer controlled power supply via platinum wire electrodes. DNA was extracted with 65% efficiency after loading lysed cells onto a silica monolith. Ethanol contained within an agarose gel matrix was then used to wash unwanted debris away from the sample by EOP (100 V cm(-1) for 5 min). The retained DNA was subsequently eluted from the monolith by water contained in a second agarose gel, again by EOP using an electric field of 100 V cm(-1) for 5 min, and transferred into the PCR reagent containing gel. The eluted DNA in solution was successfully amplified by PCR, confirming that the concept of a complete self-contained microfluidic device could be realised for DNA sample clean up and amplification, using a simple pumping and on-chip reagent storage methodology.

  4. SERI Desiccant Cooling Test Facility. Status report. Preliminary data on the performance of a rotary parallel-passage silica-gel dehumidifier

    Energy Technology Data Exchange (ETDEWEB)

    Schultz, K.J.

    1986-04-01

    This report describes the SERI Desiccant Cooling Test Facility. The facility can test bench-scale rotary dehumidifiers over a wide range of controlled conditions. We constructed and installed in the test loop a prototype parallel-passage rotary dehumidifier that has spirally wound polyester tape coated with silica gel. The initial tests gave satisfactory results indicating that approximately 90% of the silica gel was active and the overall Lewis number of the wheel was near unity. The facility has several minor difficulties including an inability to control humidity satisfactorily and nonuniform and highly turbulent inlet velocities. To completely validate the facility requires a range of dehumidifier designs. Several choices are available including constructing a second parallel-passage dehumidifier with the passage spacing more uniform.

  5. Structure and catalytic activity of metal complexes immobilized on supports. Part 1. The synthesis of palladium complexes on silica gel, modified by aldiminopropylheteryl groups, and their properties

    Energy Technology Data Exchange (ETDEWEB)

    Nesterov, M.A.; Lafer, L.I.; Dykh, Z.L.; Sharf, V.Z.; Yakerson, V.I.

    1987-07-10

    Based on silica gel containing a ..gamma..-aminopropyl group and ..cap alpha..-, ..beta..-, and ..gamma..-aldehydes of the heterocyclic series, supports having graft aldimine groups and their stable complexes with palladium have been obtained. It has been established by IR spectroscopy that the hydroxyl coating of silica gel is almost completely replaced by functional groups of ligands combined with the surface through O atoms. The Pd atom is coordinated by the N atom of the aldimine group, the heteroatom of the pyridine ring, and in the case of furan by the ..pi..-electrons of the ring. The catalytic activity and selectivity of Pd complexes in the isomerization and hydrogenation of allylbenzene is determined by the nature of the grafted heterocyclic ligand.

  6. Enhanced conductivity of sol-gel silica cladding for efficient poling in electro-optic polymer/TiO2 vertical slot waveguide modulators.

    Science.gov (United States)

    Enami, Yasufumi; Jouane, Youssef; Luo, Jingdong; Jen, Alex K-Y

    2014-12-01

    We report the enhanced conductivity of sol-gel silica under-cladding for efficient poling of electro-optic (EO) polymer in a hybrid EO polymer/TiO2 vertical slot waveguide modulator. The electrical volume conductivity of sol-gel silica cladding increases approximately 30 times when the calcining time of the cladding layer is critically reduced to 45 minutes, which increases the in-device EO coefficient of the 600-nm-thick EO polymer film in modulators and reduces the lower halfwave voltage (Vπ) of the modulators. The lowest driving voltage (Vπ) of the TiO2 slot waveguide modulator is 2.0 V for an electrode length (Le) of 10 mm and wavelength of 1550 nm (VπLe = 2.0 V·cm) for the low-index guest-host EO polymer SEO125. The optical propagation loss is reduced to 7 dB/cm.

  7. Silica gel-assisted solvothermal production of CdS,CuxS(x=1,2) and ZnS with different morphologies

    Institute of Scientific and Technical Information of China (English)

    Titipun THONGTEM; Chalermchai PILAPONG; Somchai THONGTEM

    2009-01-01

    CdS, CuxS (x=1, 2) and ZnS with different morphologies were produced by the solvothermal reactions of M(CH3COO)2'2H2O (M=Cd, Cu and Zn) and NH2CSNH2 in hexane with and without silica gel as a hard template at 200 ℃ for 24 h. The product phases were detected using X-ray diffraction (XRD). Different morphologies were characterized using a scanning electron microscope (SEM). The existence of silica gel in modeling morphologies of the sulfides was characterized using Fourier transform infrared (FTIR) spectrometer. Raman spectra of different products show the vibrations at the same wavenumbers, although they are composed of different morphologies. Photoluminescence (PL) emissions of the corresponding phases with different morphologies are at the same values, but their intensities are increased by template adding.

  8. Remaining Sites Verification Package for the 100-F-44:4, Discovery Pipeline in Silica Gel Pit, Waste Site Reclassification Form 2008-030

    Energy Technology Data Exchange (ETDEWEB)

    J. M. Capron

    2008-09-23

    The 100-F-44:4, Discovery Pipeline in Silica Gel Pit subsite is located in the 100-FR-1 Operable Unit of the Hanford Site, near the location of the former 110-F Gas Storage Tanks structure. The 100-F-44:4 subsite is a steel pipe discovered October 17, 2004, during trenching to locate the 118-F-4 Silica Gel Pit. Based on visual inspection and confirmatory investigation sampling data, the 100-F-44:4 subsite is a piece of non-hazardous electrical conduit debris. The 100-F-44:4 subsite supports unrestricted future use of shallow zone soil and is protective of groundwater and the Columbia River. No residual contamination exists within the deep zone. Therefore, no deep zone institutional controls are required.

  9. Preparation of Scratch-Resistant Nano-Porous Silica Films Derived by Sol-Gel Process and Their Anti-reflective Properties

    Institute of Scientific and Technical Information of China (English)

    Guangming WU; Jun SHEN; Tianhe YANG; Bin ZHOU; Jue WANG

    2003-01-01

    Structural strengthening of the nano porous silica films has been reported. The films were prepared with a base/acid two-step catalyzed TEOS-based sol-gel processing and dip-coating, and then baked in the mixed gas of ammonia and water vapor. The silica films were characterized with TEM, AFM, FTIR, spectrophotometer, ellipsometer, and abrasion test, respectively. The experimental results have shown that the films have a nanostructure with a low refractive index and can form an excellent scratch-resistant broadband anti-reflectance. The two-step catalysis noticeably strengthens the films, and the mixed gas treatment further improves mechanical strength of the silica network. Finally the strengthening mechanism has been discussed.

  10. Reaction Kinetics of LiOH Improved with Composite Silica Gel of Lanthanum Chloride for Absorbing CO2

    Institute of Scientific and Technical Information of China (English)

    Zhao Zhuo; Fu Pingfeng; Wang Jingxin

    2007-01-01

    A static method was employed to study the reaction kinetics of anhydrous lithium hydroxide (LiOH) and CO2. The reaction generated water was absorbed with the composite silica gel of lanthanum chloride to make the experiment repeatable. At the reaction temperature of 15~60℃ and initial CO2 pressures of 25~100kPa, the reaction rate of anhydrous LiOH and CO2 decreased slightly with the reduction of initial CO2 pressure and the rise of reaction temperature, indicating that the reaction activation energy of LiOH and CO2 was negative and close to zero. During the middle period (1~5 min) of the isothermal reaction, the ratio of reaction efficiency was approximately the power of 0.4 to that of initial CO2 pressures. As anhydrous LiOH reacted to CO2, the solid product Li2CO3 covered on the surface of LiOH was not compact, so it did not hinder the subsequent reaction of absorbing the CO2 gas. The reaction kinetics of anhydrous LiOH and CO2 obeyed the Erofeev's model.

  11. Preparation and adsorption behavior of berberine hydrochloride imprinted polymers by using silica gel as sacrificed support material

    Science.gov (United States)

    Li, Hui; Li, Yuzhuo; Li, Zhiping; Peng, Xiyang; Li, Yanan; Li, Gui; Tan, Xianzhou; Chen, Gongxi

    2012-03-01

    Preparation of berberine hydrochloride (B-Cl) imprinted polymers (MIPs) based on surface imprinting technique with silica gel as sacrificial support material was performed successfully by using B-Cl as template, methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) as functional monomer and cross-linker, respectively. The prepared polymers were characterized by Fourier transmission infrared spectrometry (FTIR) and scanning electron microscopy (SEM). Adsorption behavior of the MIPs for the template and its structural analogues was investigated. Sites distribution on the surface of MIPs was explored by using different isotherm adsorption models and thermodynamic parameters for the adsorption of B-Cl on the MIPs determined. Sample application and reusability for the MIPs was also evaluated. Results indicated the strong adsorption and high selectivity of the MIPs for B-Cl. Saturated adsorption capacity reached 27.2 μmol g-1 and the selectivity coefficient of the MIPs for B-Cl relative to jatrorrhizine hydrochloride (J-Cl) and palmatine palmatus hydrochloride (P-Cl) are 3.70 and 6.03, respectively. In addition, the MIPs were shown with good reusability and selectively retention ability in sample application.

  12. Preparation and adsorption behavior of berberine hydrochloride imprinted polymers by using silica gel as sacrificed support material

    Energy Technology Data Exchange (ETDEWEB)

    Li Hui, E-mail: lihuijsdx@163.com [Key Laboratory of Plant Resource Conservation and Utilization, Jishou University, Hunan Jishou, 416000 (China); Li Yuzhuo [Key Laboratory of Plant Resource Conservation and Utilization, Jishou University, Hunan Jishou, 416000 (China); Li Zhiping [College of Chemistry and Chemical Engineering, Jishou University, Hunan Jishou, 416000 (China); Peng Xiyang; Li Yanan; Li Gui; Tan Xianzhou; Chen Gongxi [Key Laboratory of Plant Resource Conservation and Utilization, Jishou University, Hunan Jishou, 416000 (China)

    2012-03-01

    Preparation of berberine hydrochloride (B-Cl) imprinted polymers (MIPs) based on surface imprinting technique with silica gel as sacrificial support material was performed successfully by using B-Cl as template, methacrylic acid (MAA) and ethylene glycol dimethacrylate (EGDMA) as functional monomer and cross-linker, respectively. The prepared polymers were characterized by Fourier transmission infrared spectrometry (FTIR) and scanning electron microscopy (SEM). Adsorption behavior of the MIPs for the template and its structural analogues was investigated. Sites distribution on the surface of MIPs was explored by using different isotherm adsorption models and thermodynamic parameters for the adsorption of B-Cl on the MIPs determined. Sample application and reusability for the MIPs was also evaluated. Results indicated the strong adsorption and high selectivity of the MIPs for B-Cl. Saturated adsorption capacity reached 27.2 {mu}mol g{sup -1} and the selectivity coefficient of the MIPs for B-Cl relative to jatrorrhizine hydrochloride (J-Cl) and palmatine palmatus hydrochloride (P-Cl) are 3.70 and 6.03, respectively. In addition, the MIPs were shown with good reusability and selectively retention ability in sample application.

  13. Characteristics and Laser Performance of Yb3+-Doped Silica Large Mode Area Fibers Prepared by Sol–Gel Method

    Directory of Open Access Journals (Sweden)

    Shikai Wang

    2013-12-01

    Full Text Available Large-size 0.1 Yb2O3–1.0 Al2O3–98.9 SiO2 (mol% core glass was prepared by the sol–gel method. Its optical properties were evaluated. Both large mode area double cladding fiber (LMA DCF with core diameter of 48 µm and large mode area photonic crystal fiber (LMA PCF with core diameter of 90 µm were prepared from this core glass. Transmission loss at 1200 nm is 0.41 dB/m. Refractive index fluctuation is less than 2 × 10−4. Pumped by 976 nm laser diode LD pigtailed with silica fiber (NA 0.22, the slope efficiency of 54% and “light-to-light” conversion efficiency of 51% were realized in large mode area double cladding fiber, and 81 W laser power with a slope efficiency of 70.8% was achieved in the corresponding large mode area photonic crystal fiber.

  14. Polymer particles filled with multiple colloidal silica via in situ sol-gel process and their thermal property

    Science.gov (United States)

    Byun, Hongsik; Hu, Jiayun; Pakawanit, Phakkhananan; Srisombat, Laongnuan; Kim, Jun-Hyun

    2017-01-01

    The in situ formation of dielectric silica (SiO2) particles was carried out in the presence of temperature-responsive poly(N-isopropylacrylamide) particles. Unlike the typical sol-gel method used to prepare various SiO2 particles, the highly uniform growth of SiO2 particles was achieved within the cross-linked polymer particles (i.e., the polymer particles were filled with the SiO2 particles) simply by utilizing interfacial interactions, including the van der Waals attractive force and hydrogen bonding in nanoscale environments. The structural and morphological features as well as the thermal behaviors of these composites were thoroughly examined by electron microscopes, dynamic light scattering, and thermal analyzers. In particular, the thermal properties of these composites were completely different from the bare polymer, SiO2 particles, and their mixtures, which clearly suggested the successful incorporation of multiple SiO2 particles within the cross-linked polymer particles. Similarly, titanium oxide (TiO2) particles were easily embedded within the polymer particle template which exhibited improved overall properties. As a whole, understanding in situ formation of nanoscale inorganic particles within polymer particle templates can allow for designing novel composite materials possessing enhanced chemical and physical properties.

  15. Direct electrochemical immunoassay based on a silica nanoparticles/sol-gel composite architecture for encapsulation of immunoconjugate.

    Science.gov (United States)

    Wang, Fu-Chang; Yuan, Ruo; Chai, Ya-Qin

    2006-10-01

    A highly hydrophobic and non-toxic colloidal silica nanoparticle/polyvinyl butyral sol-gel composite membrane was prepared on a platinum wire electrode. With diphtheria-toxoid (D-Ag) as a model antigen and encapsulation of diphtheria antibody (D-Ab) in the composite architecture, this membrane could be used for reagentless electrochemical immunoassay. It displayed a porous and homogeneous composite architecture without the aggregation of the immobilized protein molecules. The formation of immunoconjugate by a simple one-step immunoreaction between D-Ag in sample solution and the immobilized D-Ab introduced the change in the potential. Under optimal conditions, the D-Ag analyte could be determined in the linear ranges from 10 to 800 ng ml(-1) with a relatively low detection limit of 2.3 ng ml(-1) at 3delta. The D-Ag immunosensor exhibited good precision, high sensitivity, acceptable stability, accuracy, and reproducibility. This composite membrane could be used efficiently for the entrapment of different biomarkers and clinical applications.

  16. Reaction Kinetics of LiOH· H2O and CO2 Improved with Composite Silica Gel of Lanthanum Chloride

    Institute of Scientific and Technical Information of China (English)

    Zhao Zhuo; Fu Pingfeng; Wang Jingxin

    2007-01-01

    Reaction kinetics of LiOH·H2O and C·2 within a closed system were studied under the adsorption of water vapor by composite silica gel of lanthanum chloride. At the reaction temperature of 273~323K and initial CO2 pressures of 40~100kPa, reaction kinetics obeyed the Erofeev model. The reaction rate decreased slightly while the initial CO2 pressure reduced. When the reaction occurred at 273~299K, the reaction rate was so low that it was almost independent of the reaction temperature. However, as the temperature rose up to 300~323K, LiOH·H2O dehydrated its crystal water, and both the dehydrated and reaction-generated water were evaporated from solid reactant. For the dehydration rate increased, the reaction rate also increased as the reaction temperature rose. While the temperature was higher than 323K, the reaction apparent activation energy of LiOH·H2O and CO2, was higher than 52.5kJ·mol-1 and close to 61.4kJ·mol-1 of the LiOH·H2O dehydrated enthalpy variable at 298K, in which anhydrous LiOH was the major reactant and showed the reaction characteristics of LiOH crystals.

  17. Cobalt(II phthalocyanine bonded to 3-n-propylimidazole immobilized on silica gel surface: preparation and electrochemical properties

    Directory of Open Access Journals (Sweden)

    Fujiwara Sergio T.

    1999-01-01

    Full Text Available Co-Phthalocyanine complex was immobilized on 3-n-propylimidazole groups grafted on a porous SiO2 surface (specific surface area S BET = 500 m² g-1 and efficiently electrocatalyzed the oxalic acid oxidation on a carbon paste electrode surface made of this material. Intermolecular interactions of the complex species which can normally interfere in the redox process practically are not observed in the present case because of a low average surface density, delta = 4.7 x 10-13 mol cm-2 (delta = Nf/S BET, where Nf is the amount of adsorbed Co-phtalocyanine per gram of modified silica gel of the complex species material prepared. The linear response of the electrode to oxalic acid concentration, between 6.5 x 10-4 and 3.2 x 10-3 mol L-1, associated with its high chemical stability makes the covalently immobilized Co-phtalocyanine complex material very attractive in preparing a new class of chemical sensors.

  18. An abrasion-resistant and broadband antireflective silica coating by block copolymer assisted sol-gel method.

    Science.gov (United States)

    Zou, Liping; Li, Xiaoguang; Zhang, Qinghua; Shen, Jun

    2014-09-02

    A double-layer broadband antireflective (AR) coating was prepared on glass substrate via sol-gel process using two kinds of acid-catalyzed TEOS-derived silica sols. The relative dense layer with a porosity of ∼10% was obtained from an as-prepared sol, while the porous layer with a porosity of ∼55% was from a modified one with block copolymer (BCP) Pluronic F127 as template which results in abundant ordered mesopores. The two layers give rise to a reasonable refractive index gradient from air to the substrate and thus high transmittance in a wide wavelength range, and both of them have the same tough skeleton despite different porosity, for which each single-layer and the double-layer coatings all behaved well in the mechanical property tests. The high transmittance and the strong ability of resisting abrasion make this coating promising for applications in some harsh conditions. In addition, the preparation is simple, low-cost, time-saving, and flexible for realizing the optical property.

  19. Synthesis of Bioactive Chlorogenic Acid-Silica Hybrid Materials via the Sol-Gel Route and Evaluation of Their Biocompatibility.

    Science.gov (United States)

    Catauro, Michelina; Pacifico, Severina

    2017-07-21

    Natural phenol compounds are gaining a great deal of attention because of their potential use as prophylactic and therapeutic agents in many diseases, as well as in applied science for their preventing role in oxidation deterioration. With the aim to synthetize new phenol-based materials, the sol-gel method was used to embed different content of the phenolic antioxidant chlorogenic acid (CGA) within silica matrices to obtain organic-inorganic hybrid materials. Fourier transform infrared (FTIR) measurements were used to characterize the prepared materials. The new materials were screened for their bioactivity and antioxidant potential. To this latter purpose, direct DPPH (2,2-diphenyl-1-picrylhydrazyl) and ABTS (2,2'-azinobis-(3-ethylbenzothiazolin-6-sulfonic acid) methods were applied: radical scavenging capability appeared strongly dependent on the phenol amount in investigated hybrids, and became pronounced, mainly toward the ABTS radical cation, when materials with CGA content equal to 15 wt% and 20 wt% were analyzed. The in vitro biocompatibility of the synthetized materials was estimated by using the MTT assay towards fibroblast NIH 3T3 cells, human keratinocyte HaCaT cells, and the neuroblastoma SH-SY5Y cell line. As cell viability and morphology of tested cell lines seemed to be unaffected by new materials, the attenuated total reflectance (ATR)-FTIR method was applied to deeply measure the effects of the hybrids in the three different cell lines.

  20. Selective extraction and detection of noble metal based on ionic liquid immobilized silica gel surface using ICP-OES

    Indian Academy of Sciences (India)

    HADI M MARWANI; AMJAD E ALSAFRANI; HAMAD A AL-TURAIF; ABDULLAH M ASIRI; SHER BAHADAR KHAN

    2016-08-01

    In this study, an efficiently employed ionic liquid combined with commercially available silica gel (SG–ClPrNTf$_2$) was developed for selective detection of gold(III) by use of inductively coupled plasma–optical emission spectrometry (ICP-OES). The selectivity of SG–ClPrNTf$_2$ was evaluated towards seven metal ions, including Y(III), Mn(II), Zr(IV), Pb(II), Mg(II), Pd(II) and Au(III). Based on pH study and distribution coefficient values, the SG–ClPrNTf$_2$ phase was found to be the most selective towards Au(III) at pH 2 as compared to other metal ions. The adsorption isotherm of Au(III) on the SG–ClPrNTf$_2$ phase followed the Langmuir model with adsorption capacity of 59.48 mg g$^{−1}$, which was highly in agreement with experimental data of adsorption isotherm study. The kinetics study indicated that Au(III) adsorption kinetics data were well fit with the pseudo-second-order kinetic model on the basis of correlation coefficient fitting (0.996) and adsorption capacity agreement (62.26 mg g$^{−1}$). Furthermore, SG–ClPrNTf$_2$ phase was effectively performed for the determination of Au(III) in real water samples with satisfactory results.

  1. Determination of lead, iron and nickel in water and vegetable samples after preconcentration with aspergillus niger loaded on silica gel

    Energy Technology Data Exchange (ETDEWEB)

    Baytak, Sitki [Harran University, Arts and Science Faculty, Department of Chemistry, Sanliurfa (Turkey); Kocyigit, Abdurrahim [Harran University, Faculty of Medicine, Department of Biochemistry, Sanliurfa (Turkey); Rehber Tuerker, Ali [Gazi University, Arts and Science Faculty, Department of Chemistry, Ankara (Turkey)

    2007-12-15

    A method for the determination of Fe(III), Pb(II), and Ni(II) by flame atomic absorption spectrometry (FAAS) after preconcentrating on a column containing Aspergillus niger loaded on silica gel 60 (Biosorbent) is described. The effect of experimental parameters such as pH, flow rate of sample solution, and volume of sample solution were investigated on the recovery of the analytes. The effect of interfering ions on the recovery of the analytes has also been investigated. Recoveries of Fe(III), Pb(II), and Ni(II) were (98 {+-} 2), (98 {+-} 3), (99 {+-} 2)% at the 95% confidence level, respectively. For the analytes, 50-fold preconcentration was obtained. The analytical detection limits for Fe(III), Pb(II), and Ni(II) were 1.7, 5.2, and 1.6 ng/mL, respectively. The proposed method was applied to the determination of trace metals in various water and vegetable samples. The analytes have been determined with relative error lower than 7%. (Abstract Copyright [2007], Wiley Periodicals, Inc.)

  2. Immobilization of Chiral Ferrocenyl Ligands on Silica Gel and their Testing in Pd-catalyzed Allylic Substitution and Rh-catalyzed Hydrogenation

    Directory of Open Access Journals (Sweden)

    Duncan J. Macquarrie

    2005-07-01

    Full Text Available Five different silica gels containing two chiral ferrocenyl ligands were prepared by various synthetic routes and tested in an enantioselective Pd(0-catalyzed allylic substitution and Rh-catalyzed hydrogenation. All the prepared anchored ligands were characterized by porosimetry data, DRIFTS spectra, thermal data and AAS. The aim of the work was to compare the influence of the carrier, surface properties and immobilization strategy on the performance of the catalyst.

  3. X-ray diffraction line profile analysis of nano-sized cobalt in silica matrix synthesized by sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Sen, Ranjan, E-mail: ranjansen2001@gmail.co [Department of Metallurgical and Materials Engineering, Jadavpur University, Kolkata 700032 (India); Das, Gopes Chandra; Mukherjee, Siddhartha [Department of Metallurgical and Materials Engineering, Jadavpur University, Kolkata 700032 (India)

    2010-02-04

    Nano-sized cobalt particles in silica matrix have been synthesized by sol-gel method to reduce the oxidation of metallic cobalt. Different techniques of the X-ray diffraction line profile analysis (XRDLPA) have been used to determine the microstructural parameters of the nano-sized cobalt. The domain size, microstrain and lattice parameters have been estimated by the modified Rietveld technique and classical Williamson-Hall technique.

  4. Effect of the Silanization Conditions on Chromatographic Behavior of an Open-tubular Capillary Column Coated with a Modified Silica-gel Thin Layer

    OpenAIRE

    Yusuke, Nakano; Shinya, Kitagawa; Kanji, Miyabe; Takao, Tsuda

    2005-01-01

    The performance of an open-tubular capillary column coated with a modified silica-gel thin layer was investigated, particularly concerning the effect of the silanization process on it. Although the increase in the octadecyltriethoxysilane (ODTES) concentration in the silanization process could enhance the retention factor of naphthalene, its theoretical plate number was significantly reduced (ODTES, 5 to 50%; k, 0.2 to 4.3; N, 79600 to 2600 m-1). Namely, the increase in the retention factor w...

  5. Effect of ZrN coating by magnetron sputtering and sol-gel processed silica coating on titanium/porcelain interface bond strength.

    Science.gov (United States)

    Xia, Yang; Zhou, Shu; Zhang, Feimin; Gu, Ning

    2011-02-01

    In this study, a coating technique was applied to improve the bond strength of titanium (Ti) porcelain. ZrN coating was prepared by magnetron sputtering, and silica coating was processed by a sol-gel method. The treated surfaces of the specimens were analyzed by X-ray diffraction, and the Ti/porcelain interface was investigated by scanning electron microscopy (SEM) and energy dispersive spectroscopy. The coated specimens appeared fully coherent to the Ti substrate. The fractured bonding surface was also investigated by SEM. The residual porcelain on the metal surface could be observed in the ZrN group and silica group, but there was no obvious porcelain remaining in the control group. A three-point-bending test showed that the bonding strength of the ZrN group (45.99 ± 0.65 MPa) was higher than the silica group (37.77 ± 0.78 MPa) (P coatings resulted in a stronger Ti/porcelain bond. ZrN coating by magnetron sputtering was a more effective way to improve the bond strength between Ti and porcelain compared with sol-gel processed silica coating in this study.

  6. Adsorption of Pb(II) using silica gel composite from rice husk ash modified 3-aminopropyltriethoxysilane (APTES)-activated carbon from coconut shell

    Science.gov (United States)

    Yusmaniar, Purwanto, Agung; Putri, Elfriyana Awalita; Rosyidah, Dzakiyyatur

    2017-03-01

    Silica gel modified by 3-aminopropyltriethoxysilane (APTES) was synthesized from rice husk ash combined with activated carbon from coconut shell yielded the composite adsorbent. The composite was characterized by Fourier Transform Infra Red spectroscopy (FT-IR), Electron Dispersive X-Ray (EDX), Surface Area Analyzer (SAA) and adsorption test by Atomic Absorption Spectrometry (AAS). This composite adsorbent has been used moderately for the removal of lead ions from metal solutions and compared with silica gel modified APTES and activated carbon. The adsorption experiments of Pb -ions by adsorbents were performed at different pH and contact time with the same metal solutions concentration, volume solution, and adsorbent dosage. The optimum pH for the adsorption was found to be 5.0 and the equilibrium was achieved for Pb with 20 min of contact time. Pb ions adsorption by composite silica gel modified APTES-activated carbon followed by Langmuir isotherm model with qmax value of 46.9483 mg/g that proved an adsorbent mechanism consistent to the mechanism of monolayer formation.

  7. Preconcentration and separation of copper(II), cadmium(II) and chromium(III) in a syringe filled with 3-aminopropyltriethoxysilane supported on silica gel.

    Science.gov (United States)

    Tokman, Nilgun; Akman, Suleyman; Ozcan, Mustafa; Koklu, Unel

    2002-11-01

    In this study, a syringe was filled with silica gel loaded with 3-aminopropyltriethoxysilane, for the separation and preconcentration of copper, cadmium and chromium prior to their determination by graphite furnace atomic absorption spectrometry (GFAAS) in seawater. For this purpose, a syringe was filled with 0.5 g of modified silica gel and the sample solution was drawn into the syringe and ejected back again. The analyte elements were quantitatively retained at pH 5. Then, the elements sorbed by the silica gel were eluted with 2.0 M of HCl and determined by GFAAS. At optimum conditions, the recovery of Cu, Cd and Cr were 96-98%. Detection limits (3delta) were 6.6, 7.5 and 6.0 micro g L(-1) for Cu, Cd and Cr, respectively. The elements could be concentrated by drawing and discharging several portions of sample successively but eluting only once. Cu, Cd and Cr added to a seawater sample were quantitatively recovered (>95%) in the range of the 95% confidence level. The method proposed in this paper was compared with a column technique. Optimum experimental conditions, reproducibility, precision and recoveries of both techniques are the same, but the syringe technique is much faster, easier and more practical than the column technique. It is a portable system and allows one to make the sorption process in the source of sample. In addition, the risk of contamination is less than in the column technique.

  8. Comparison of sulfuric acid treatment and multi-layer silica gel column chromatography in cleanup methods for determination of PCDDs, PCDFs and dioxin-like PCBs in foods.

    Science.gov (United States)

    Amakura, Yoshiaki; Tsutsumi, Tomoaki; Sasaki, Kumiko; Toyoda, Masatake; Maitani, Tamio

    2002-10-01

    Two typical cleanup methods, sulfuric acid treatment and multi-layer silica gel column chromatography, for the determination of polychlorinated dibenzo-p-dioxins (PCDDs), dibenzofurans (PCDFs) and dioxin-like polychlorinated biphenyls (dioxin-like PCBs) in seventeen food samples were examined and compared. Vegetables, fruits, cereals, fish, meat and dairy foods were extracted by conventional methods (shaking with acetone/n-hexane or with n-hexane after alkaline treatment). The extracts were cleaned up by sulfuric acid treatment or multi-layer silica gel column chromatography, followed by several column chromatographic steps. Of the samples treated, the vegetable, fruit and cereal samples could be directly applied to the multi-layer silica gel column after extraction. However, the samples containing fats and oils such as fish, meat and dairy foods needed to be treated several times with concentrated sulfuric acid before multi-layer column chromatography, because these samples plugged the column with oily residues. Both cleanup methods gave similar values of isomeric concentrations and showed similar efficiency of purification, and the recoveries ranged from 40 to 120%. These results are considered to provide useful data for the efficient analysis of dioxins in foods which have wide-ranging compositions.

  9. Densitometric HPTLC method for qualitative, quantitative analysis and stability study of Coenzyme Q10 in pharmaceutical formulations utilizing normal and reversed-phase silica gel plates.

    Science.gov (United States)

    Abdel-Kader, Maged Saad; Alam, Prawez; Alqasoumi, Saleh Ibrahim

    2016-03-01

    Two simple, precise and stability-indicating densitometric HPTLC method were developed and validated for qualitative and quantitative analysis of Coenzyme Q10 in pharmaceutical formulations using normal-phase (Method I) and reversed phase (Method II) silica gel TLC plates. Both methods were developed and validated with 10×20 cm glass-backed plates coated with 0.2 mm layers of either silica gel 60 F254 (E-Merck, Germany) using hexane-ethyl acetate (8.5:1.5 v/v) as developing system (Method I) or RP-18 silica gel 60 F254 (E-Merck, Germany) using methanol-acetone (4:6 v/v) as mobile phase (Method II). Both analyses were scanned with a densitometer at 282 nm. Linearity was found in the ranges 50-800 ng/spot (r(2)=0.9989) and 50-800 ng/spot (r(2)=0.9987) for Method I and Method II respectively. Stability of Coenzyme Q10 was explored by the two methods using acid, base, hydrogen peroxide, temperature and different solvents. Due to the efficiency of the method in separating Coenzyme Q10 from other ingredients including its degradation products, it can be applied for quality control, standardization of different pharmaceutical formulations and stability study.

  10. Obtaining of Sol-Gel Ketorolac-Silica Nanoparticles: Characterization and Drug Release Kinetics

    Directory of Open Access Journals (Sweden)

    T. M. López Goerne

    2013-01-01

    Full Text Available Nonsteroidal anti-inflammatory drugs (NSAIDs are among most commonly prescribed medications worldwide. NSAIDs play an important role due to their pronounced analgesic potency, anti-inflammatory effects, and lesser side effects compared to opioids. However, adverse effects including gastrointestinal and cardiovascular effects seriously complicate their prolonged use. In the present work we prepare SiO2-based nanoparticles with ketorolac, for controlled release proposes. The nanomaterials were prepared by the sol-gel technology at acidic conditions and two different water/alcoxide ratios were used. FTIR spectroscopy was performed in order to characterize the solids and drug-SiO2 interactions. Thermal analysis and nitrogen adsorption isotherms showed thermal stability of the drug and confirmed the presence of particles with high surface area. Transmission electron micrographies of the samples showed the nanosize particles (20 nm forming aggregates. Drug release profiles were collected by means of UV-Vis spectroscopy and kinetic analysis was developed. Release data were fitted and 1 : 8 sample showed a sustained release over ten hours; 90% of the drug was delivered at the end of the time.

  11. Covalently anchored sulfonic acid on silica gel (SiO2-R-SO3H) as an efficient and reusable heterogeneous catalyst for the one-pot synthesis of 1,8-dioxooctahydroxanthenes under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Gholam Hossein Mahdavinia; Mohammad A.Bigdeli; Yaser Saeidi Hayeniaz

    2009-01-01

    A highly efficient one-pot synthesis of 1,8-dioxooctahydroxanthenes under solvent-free conditions catalyzed by sulfonic acid covalently anchored onto the surface of silica gel is reported.All types of aldehydes,including aromatic,unsaturated,and heterocyclic,are used.The silica gel/sulfonic acid catalyst (SiO2-R-SO3H) is completely heterogeneous and can be recycled.

  12. Organic-inorganic crosslinked and hybrid membranes derived from sulfonated poly(arylene ether sulfone)/silica via sol-gel process

    Science.gov (United States)

    Feng, Shaoguang; Shang, Yuming; Wang, Yingzi; Xie, Xiaofeng; Mathur, V. K.; Xu, Jingming

    A series of covalently crosslinkable organic-inorganic hybrid membranes have been prepared from sulfonated poly(arylene ether sulfone) (SPAES) with pendant propenyl moiety and various amounts of vinyl substituted silica via sol-gel process which are then thermally crosslinked in the presence of benzoyl peroxide (BPO) initiator. The obtained membranes are characterized in terms of oxidative stability, thermal property, ion exchange capacity (IEC), water uptake, swelling ratio in methanol aqueous solution, proton conductivity, and methanol permeability coefficient. The results indicate that the oxidative stability and thermal stability of the hybrid membranes are improved. Moreover, introduction of silica reduces the water uptake and methanol swelling of membranes. The swelling ratio of membranes in 2 mol L -1 methanol aqueous solution at 80 °C slowly decreases from 26 to 19% with the increase of SiO 2 content from 0 to 12 wt.%. Furthermore, with the increase in silica content, the methanol permeability coefficient of the hybrid membranes decreases at first and then increases. When the silica content reaches 8 wt.%, the methanol permeability coefficient is at the minimum of 6.02 × 10 -7 cm 2 s -1, a 2.64-fold decrease compared with that of the pristine SPAES membrane. Moreover, the proton conductivity is found to be at about 95% of that of pristine polymer at that silica content.

  13. Effect of the size of silica nanoparticles on wettability and surface chemistry of sol-gel superhydrophobic and oleophobic nanocomposite coatings

    Science.gov (United States)

    Lakshmi, R. V.; Bera, Parthasarathi; Anandan, C.; Basu, Bharathibai J.

    2014-11-01

    Superhydrophobic sol-gel nanocomposite coatings have been fabricated by incorporating silica nanoparticles with different particle sizes separately in an acid-catalyzed sol of methyltriethoxysilane (MTEOS). Water contact angle (WCA) of the coatings increased with increase in the concentration of silica nanoparticles in both the cases. The coatings became superhydrophobic at an optimum silica concentration. The water repellency was further improved by the addition of fluoroalkylsilane (FAS). The optimum silica concentration was found to depend on the size of silica nanoparticles and FAS content and the coatings exhibited WCA of about 160° and water sliding angle (WSA) of oleophobicity of the coatings. The coatings exhibited oil-repellency with a lubricant oil contact angle of 126° and ethylene glycol contact angle of 153.3°. Surface morphology of the coatings analyzed using field emission scanning electron microscopy (FESEM) showed a rough surface with microscale bumps and nanoscale pores. XPS was used to study the surface composition of the coatings. The superhydrophobic property of the coatings was due to the synergistic effect of surface chemistry and surface microstructure and can be explained using Cassie-Baxter model.

  14. Organic-inorganic crosslinked and hybrid membranes derived from sulfonated poly(arylene ether sulfone)/silica via sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Feng, Shaoguang; Shang, Yuming; Wang, Yingzi; Xie, Xiaofeng; Xu, Jingming [Institute of Nuclear and New Energy Technology, Tsinghua University, Beijing 100084 (China); Mathur, V.K. [Department of Chemical Engineering, University of New Hampshire, NH 03824 (United States)

    2010-05-01

    A series of covalently crosslinkable organic-inorganic hybrid membranes have been prepared from sulfonated poly(arylene ether sulfone) (SPAES) with pendant propenyl moiety and various amounts of vinyl substituted silica via sol-gel process which are then thermally crosslinked in the presence of benzoyl peroxide (BPO) initiator. The obtained membranes are characterized in terms of oxidative stability, thermal property, ion exchange capacity (IEC), water uptake, swelling ratio in methanol aqueous solution, proton conductivity, and methanol permeability coefficient. The results indicate that the oxidative stability and thermal stability of the hybrid membranes are improved. Moreover, introduction of silica reduces the water uptake and methanol swelling of membranes. The swelling ratio of membranes in 2 mol L{sup -1} methanol aqueous solution at 80 C slowly decreases from 26 to 19% with the increase of SiO{sub 2} content from 0 to 12 wt.%. Furthermore, with the increase in silica content, the methanol permeability coefficient of the hybrid membranes decreases at first and then increases. When the silica content reaches 8 wt.%, the methanol permeability coefficient is at the minimum of 6.02 x 10{sup -7} cm{sup 2} s{sup -1}, a 2.64-fold decrease compared with that of the pristine SPAES membrane. Moreover, the proton conductivity is found to be at about 95% of that of pristine polymer at that silica content. (author)

  15. Enhanced Photophysical Properties of Nanopatterned Titania Nanodots/Nanowires upon Hybridization with Silica via Block Copolymer Templated Sol-Gel Process

    Directory of Open Access Journals (Sweden)

    Dinakaran Kannaiyan

    2010-10-01

    Full Text Available We fabricated titanium dioxide (TiO2-silica (SiO2 nanocomposite structures with controlled morphology by a simple synthetic approach using cooperative sol-gel chemistry and block copolymer (BCP self-assembly. Mixed TiO2-SiO2 sol-gel precursors were blended with amphiphilic poly(styrene-block-ethylene oxide (PS-b-PEO BCPs where the precursors were selectively incorporated into the hydrophilic PEO domains. Changing the volumetric ratio of TiO2-SiO2 sol-gel precursor from 5% to 20%, a stepwise structural inversion occurred from nanodot arrays to discrete nanowires. Template free hybrid inorganic nanostructures were produced after the removal of PS-b-PEO by irradiation of UV light. The morphological evolution and photophysical properties were investigated by microscopic studies, UV-visible absorption and photocatalytic properties.

  16. A new precursor for the immobilization of enzymes inside sol-gel-derived hybrid silica nanocomposites containing polysaccharides.

    Science.gov (United States)

    Shchipunov, Yurii A; Karpenko, Tat'yana Yu; Bakunina, Irina Yu; Burtseva, Yuliya V; Zvyagintseva, Tat'yana N

    2004-01-30

    Tetrakis(2-hydroxyethyl) orthosilicate (THEOS) introduced by Hoffmann et al. (J. Phys. Chem. B., 106 (2002) 1528) was first used to prepare hybrid nanocomposites containing various polysaccharides and immobilize enzymes in these materials. Two different types of O-glycoside hydrolyses (EC3.2.1), 1-->3-beta-D-glucanase LIV from marine mollusk Spisula sacchalinensis and alpha-D-galactosidase from marine bacterium Pseudoalteromonas sp. KMM 701, were taken for the immobilization. To reveal whether the polysaccharide inside the hybrid material influences the enzyme entrapment and functioning, negatively charged xanthan, cationic derivative of hydroxyethylcellulose and uncharged locust bean gum were examined. The mechanical properties of these nanocomposites were characterized by a dynamic rheology and their structure by a scanning electron microscopy. It was found that 1-->3-beta-D-glucanase was usually immobilized without the loss of its activity, while the alpha-D-galactosidase activity in the immobilized state depended on the polysaccharide type of material. An important point is that the amount of immobilized enzymes was small, comparable to their content in the living cells. It was shown by the scanning electron microscopy that the hybrid nanocomposites are sufficiently porous that allows the enzymatic substrates and products to diffuse from an external aqueous solution to the enzymes, whereas protein molecules were immobilized firmly and not easily washed out of the silica matrix. A sharp increase of the enzyme lifetime (more than a hundred times) was observed after the immobilization. As established, the efficient entrapment of enzymes is caused by few advantages of new precursor over the currently used TEOS and TMOS: (i) organic solvents and catalysts are not needed owing to the complete solubility of THEOS in water and the catalytic effect of polysaccharides on the sol-gel processes; (ii) the entrapment of enzymes can be performed at any pH which is suitable

  17. Synthesis of silica gel supported salicylaldehyde modified PAMAM dendrimers for the effective removal of Hg(II) from aqueous solution.

    Science.gov (United States)

    Niu, Yuzhong; Qu, Rongjun; Chen, Hou; Mu, Lei; Liu, Xiguang; Wang, Ting; Zhang, Yue; Sun, Changmei

    2014-08-15

    A series of silica gel supported salicylaldehyde modified PAMAM dendrimers (SiO2-G0-SA ∼ SiO2-G2.0-SA) were synthesized and their structures were characterized by FTIR, XRD, SEM, TGA, and porous structure analysis. The feasibility of these adsorbents for the removal of Hg(II) from aqueous solution was first described and the adsorption mechanism was proposed. The adsorption was found to depend on solution pH, the generation number of salicylaldehyde modified PAMAM dendrimers, contact time, temperature, and initial concentration. Results showed that the optimal pH was about 6 and the adsorption capacity increased with the increasing of generation number. Density functional theory (DFT) method was used to investigate the coordination geometries and the chelating mechanism. Adsorption kinetics was found to follow the pseudo-second-order model with film diffusion process as rate controlling step. Adsorption isotherms revealed that adsorption capacities increased with the increasing of temperature. Langmuir, Freundlich and Dubinin-Radushkevich (D-R) isotherm models were employed to analyze the equilibrium data. The adsorption can be well described by Langmuir isotherm model and took place by chemical mechanism. The thermodynamics properties indicated the adsorption processes were spontaneous and endothermic nature. The maximum adsorption capacity of SiO2-G0-SA, SiO2-G1.0-SA, and SiO2-G2.0-SA were 0.91, 1.52, and 1.81 mmol g(-1), respectively. The considerable higher adsorption capacity compared with other adsorbents indicates SiO2-G0-SA ∼ SiO2-G2.0-SA are favorable and useful for the uptake of Hg (II), and can be potentially used as promising adsorbents for the effective removal of Hg(II) from aqueous solution.

  18. Distribution threshold values of CaCl2 onto the 10X-zeolite and macro-pore silica gel

    Institute of Scientific and Technical Information of China (English)

    TANG YouCheng; LI Bin; YANG JingChang; CHU Wei; LUO ShiZhong

    2009-01-01

    The calcium chloride used for adsorption separation of ammonia is promising for its large adsorptive capacity and lower desorption temperature, but difficult to develop because of the liable expansion, lump and chip in the adsorption/desorption process. Composite adsorbents made by monolayer dis-persion of calcium chloride onto carriers with high surface areas exhibit better adsorptive capacity and stability. Several models were developed to confirm the maximum monolayer dispersion capacity of calcium chloride onto the carriers (the distribution threshold value), and the closely packed monolayer dispersion model was considered the most suitable for this study. The distribution threshold values given by this model were 0.60 g CaCl2/(g 10X-zeolite) and 0.38 g CaCl2/(g SiO2). When the divalent salt was dispersed onto the carriers, however, anions were separated into two types, causing that the en-tropy of the system tended to increase and the system was not stable. To minimize the entropy, a new model was put forward as the modified closely packed monolayer dispersion model. Based on this model, the distribution threshold values are 0.52 g CaCl2/(g 10X-zeolite) and 0.33 g CaCl2/(g SiO2), re-spectively. The distribution threshold values were also gained experimentally by XRD quantitative phase analysis: 0.61 g CaCl2/(g 10X-zeollte) and 0.31 g CaCl2/(g SiO2). Comparison between experi-mental values of distribution threshold with theoretical ones based on two different model showed that the closely packed monolayer dispersion model fits the monolayer dispersion of calcium chloride onto micro-pore carrier -10X-zeolite, and the modified closely packed monolayer dispersion model is more suitable for the bigger aperture carrier -macro-pore silica gel.

  19. Sol-gel derived silica/chitosan/Fe3O4 nanocomposite for direct electrochemistry and hydrogen peroxide biosensing

    Science.gov (United States)

    Satvekar, R. K.; Rohiwal, S. S.; Tiwari, A. P.; Raut, A. V.; Tiwale, B. M.; Pawar, S. H.

    2015-01-01

    A novel strategy to fabricate hydrogen peroxide third generation biosensor has been developed from sol-gel of silica/chitosan (SC) organic-inorganic hybrid material assimilated with iron oxide magnetic nanoparticles (Fe3O4). The large surface area of Fe3O4 and porous morphology of the SC composite facilitates a high loading of horseradish peroxidase (HRP). Moreover, the entrapped enzyme preserves its conformation and biofunctionality. The fabrication of hydrogen peroxide biosensor has been carried out by drop casting of the SC/F/HRP nanocomposite on glassy carbon electrode (GCE) for study of direct electrochemistry. The x-ray diffraction (XRD) pattern and transmission electron microscopy (TEM) confirms the phase purity and particle size of as-synthesized Fe3O4 nanoparticles, respectively. The nanocomposite was characterized by UV-vis spectroscopy, fluorescence spectroscopy and Fourier transform infrared (FTIR) for the characteristic structure and conformation of enzyme. The surface topographies of the nanocomposite thin films were investigated by scanning electron microscopy (SEM). Dynamic light scattering (DLS) was used to determine the particle size distribution. The electrostatic interactions of the SC composite with Fe3O4 nanoparticles were studied by the zeta potential measurement. Electrochemical impedance spectroscopy (EIS) of the SC/F/HRP/GCE electrode displays Fe3O4 nanoparticles as an excellent candidate for electron transfer. The SC/F/HRP/GCE exhibited a pair of well-defined quasi reversible cyclic voltammetry peaks due to the redox couple of HRP-heme Fe (III)/Fe (II) in pH 7.0 potassium phosphate buffer. The biosensor was employed to detect H2O2 with linear range of 5 μM to 40 μM and detection limit of 5 μM. The sensor displays excellent selectivity, sensitivity, good reproducibility and long term stability.

  20. Study of the interfacial stability of PVdF/HFP gel electrolytes with sub-micro- and nano-sized surface-modified silicas

    Energy Technology Data Exchange (ETDEWEB)

    Zalewska, A., E-mail: aldona@ch.pw.edu.p [Warsaw University of Technology, Department of Chemistry, Noakowskiego 3, 00-664 Warszawa (Poland); Walkowiak, M. [Institute of Non-Ferrous Metals Branch in Poznan Central Laboratory of Batteries and Cells, Forteczna 12, 61-362 Poznan (Poland); Niedzicki, L. [Warsaw University of Technology, Department of Chemistry, Noakowskiego 3, 00-664 Warszawa (Poland); Jesionowski, T. [Poznan University of Technology, Institute of Chemical Technology and Engineering, Pl. Marii Sklodowskiej-Curie 2, 60-965 Poznan (Poland); Langwald, N. [Warsaw University of Technology, Department of Chemistry, Noakowskiego 3, 00-664 Warszawa (Poland)

    2010-01-25

    The aim of the presented work was to perform a preliminary study of the physicochemical and interfacial properties of hybrid organic-inorganic gel electrolytes for Li-ion batteries based on the PVdF/HFP polymeric matrix and surface-modified silicas. Two types of silica fillers of different grain sizes (>500 nm and approx100 nm) were used as additives. The silica particles were modified by two different functional groups, i.e. methacryloxy and vinyl ones. The gel electrolytes based on PVdF/HFP copolymer were prepared according to the so-called Bellcore two-step process. The motivation of the present work was to study more deeply those systems in terms of morphology by means of scanning electron microscopy techniques. Fillers modified with identical functional groups but differing fundamentally in the manufacturing processes were compared in terms of the impact on morphology and electrochemical performance of the resulting membranes. Interfacial properties were examined by means of impedance spectroscopy technique using Swagelok-type cells with two lithium electrodes.

  1. A continuous production process for silica aerogel powders based on sodium silicate by fluidized bed drying of wet-gel slurry

    Science.gov (United States)

    Bhagat, Sharad D.; Park, Kyung-Tae; Kim, Yong-Ha; Kim, Jong-Soon; Han, Jong-Hun

    2008-09-01

    The present study described a continuous process for the production of hydrophobic silica aerogel powders based on an inexpensive precursor such as sodium silicate. Fluidization technique was employed for the drying of wet-gel slurry at an ambient pressure. The fluidization column was fed with the silylated wet-gel slurry in a continuous mode and the fluidization was carried out at 220 °C. The aerogel powder collected in Trap-I was fluidized twice at room temperature in order to separate the lighter aerogel particles from the first trap. The tapping density of the aerogel powder decreased from 0.09 to 0.05 g/cm 3 for Trap-II, however, the microstructure did not differ significantly. Using this process, hydrophobic silica aerogel powders exhibiting tapping density as low as 0.05 g/cm 3, high specific surface area of 783 m 2/g and cumulative pore volume of 1.79 cm 3/g have been obtained. The aerogels were characterized by Field-Emission Scanning Electron Microscopy (FE-SEM), BET specific surface area, N 2 physisorption isotherms, pore size distribution and particle size analyses. The results have been compared with aerogel powders obtained by ambient pressure drying of the wet-gel slurry in a furnace.

  2. A continuous production process for silica aerogel powders based on sodium silicate by fluidized bed drying of wet-gel slurry

    Energy Technology Data Exchange (ETDEWEB)

    Bhagat, Sh.D.; Park, K.T.; Kim, Y.H. [Pukyong National Univ., Faculty of Chemical Engineering, Powder Technology Lab., Busan (Korea, Republic of); Kim, J.S. [NGETECH Inc., Nam-Gu, Busan (Korea, Republic of); Han, J.H. [Korea Electronics Technology Institute, Seongnam, Gyeonggi-do (Korea, Republic of)

    2008-09-15

    The present study described a continuous process for the production of hydrophobic silica aerogel powders based on an inexpensive precursor such as sodium silicate. Fluidization technique was employed for the drying of wet-gel slurry at an ambient pressure. The fluidization column was fed with the silylated wet-gel slurry in a continuous mode and the fluidization was carried out at 220 C. The aerogel powder collected in Trap-I was fluidized twice at room temperature in order to separate the lighter aerogel particles from the first trap. The tapping density of the aerogel powder decreased from 0.09 to 0.05 g/cm{sup 3} for Trap-II, however, the microstructure did not differ significantly. Using this process, hydrophobic silica aerogel powders exhibiting tapping density as low as 0.05 g/cm{sup 3}, high specific surface area of 783 m{sup 2}/g and cumulative pore volume of 1.79 cm{sup 3}/g have been obtained. The aerogels were characterized by Field-Emission Scanning Electron Microscopy (FE-SEM), BET specific surface area, N{sub 2} physi-sorption isotherms, pore size distribution and particle size analyses. The results have been compared with aerogel powders obtained by ambient pressure drying of the wet-gel slurry in a furnace. (authors)

  3. The effect of high temperature sol-gel polymerization parameters on the microstructure and properties of hydrophobic phenol-formaldehyde/silica hybrid aerogels.

    Science.gov (United States)

    Seraji, Mohamad Mehdi; Sameri, Ghasem; Davarpanah, Jamal; Bahramian, Ahmad Reza

    2017-05-01

    Phenol-formaldehyde/silica hybrid aerogels with different degree of hydrophobicity were successfully synthesized via high temperature sol-gel polymerization. Tetraethoxysilane (TEOS) and methyltriethoxysilane (MTES) were used as precursor and co-precursor of the hydrophobic silica-based phase, respectively. The hydrolysis step of silica based sols were conducted by acid catalyzed reactions and HCl was used as hydrolysis catalyst. The chemical structure of prepared hybrid aerogels was characterized by Fourier Transform Infrared spectroscopy (FT-IR). The effect of MTES/TEOS proportion and catalyst content on the morphology and microstructure of samples were investigated by FE-SEM and C, Si mapping analysis. The acid catalyzed hydrolysis of TEOS and MTES sols leads to formation of a sol with primarily silica particles in the organic-inorganic hybrid sol and varying colloid growth mechanisms were occurred with change in MTES and HCl molar ratio. With the increasing of MTES content, the microstructure of samples changed from uniform colloidal network, core-shell structure to polymeric structure with a huge phase separation. The increasing of HCl mole fraction leads to smaller particle size. Moreover, the shrinkage of samples was decreased and water contact angles of the resulted aerogels were increased from 40 to 156.8° with the increases of MTES content.

  4. Preparation of an aminopropyl imidazole-modified silica gel as a sorbent for solid-phase extraction of carboxylic acid compounds and polycyclic aromatic hydrocarbons.

    Science.gov (United States)

    Wang, Na; Guo, Yong; Wang, Licheng; Liang, Xiaojing; Liu, Shujuan; Jiang, Shengxiang

    2014-05-21

    In this paper, a kind of aminopropyl imidazole-modified silica sorbent was synthesized and used as a solid-phase extraction (SPE) sorbent for the determination of carboxylic acid compounds and polycyclic aromatic hydrocarbons (PAHs). The resultant aminopropyl imidazole-modified silica sorbent was characterized by Fourier transform infrared spectroscopy (FT-IR) and elemental analysis (EA) to ensure the successful binding of aminopropyl imidazole on the surface of silica gel. Then the aminopropyl imidazole-modified silica sorbent served as a SPE sorbent for the enrichment of carboxylic acid compounds and PAHs. The new sorbent exhibited high extraction efficiency towards the tested compounds and the results show that such a sorbent can offer multiple intermolecular interactions: electrostatic, π-π, and hydrophobic interactions. Several parameters affecting the extraction recovery, such as the pH of sample solution, the pH of eluent, the solubility of eluent, the volume of eluent, and sample loading, were also investigated. Under the optimized conditions, the proposed method was applied to the analysis of four carboxylic acid compounds and four PAHs in environmental water samples. Good linearities were obtained for all the tested compounds with R(2) larger than 0.9903. The limits of detection were found to be in the range of 0.0065-0.5 μg L(-1). The recovery values of spiked river water samples were from 63.2% to 112.3% with relative standard deviations (RSDs) less than 10.1% (n = 4).

  5. Photocatalytic degradation for methylene blue using zinc oxide prepared by codeposition and sol-gel methods.

    Science.gov (United States)

    Shen, Wenzhong; Li, Zhijie; Wang, Hui; Liu, Yihong; Guo, Qingjie; Zhang, Yuanli

    2008-03-21

    Zinc oxide nanoparticle was obtained by zinc hydrate deposited on the silica nanoparticle surface and zinc hydrate was dispersed in starch gel. The structure of zinc oxide particle was characterized by nitrogen adsorption-desorption and XRD, the morphology was observed by TEM. The result showed that the zinc oxide nanoparticle deposited on the silica nanoparticle surface was well-dispersed and less than 50nm, displayed higher photocatalytic activity for methylene blue degradation. However, the zinc oxide nanoparticle in a size of 60nm was derived from starch gel and showed poorer photocatalytic activity. It provided a simple and effective route to prepare zinc oxide nanoparticle with higher photocatalytic activity through depositing zinc oxide on the silica particle surface, moreover, the catalyst is easier to recover due to its higher density.

  6. Evaluation of encapsulation stress and the effect of additives on viability and photosynthetic activity of Synechocystis sp. PCC 6803 encapsulated in silica gel.

    Science.gov (United States)

    Dickson, David J; Ely, Roger L

    2011-09-01

    Stresses imposed on the cyanobacterium Synechocystis sp. PCC 6803 by various compounds present during silica sol-gel encapsulation, including salt, ethanol (EtOH), polyethylene glycol (PEG), glycerol, and glycine betaine, were investigated. Viability of encapsulated cells and photosynthetic activity of cells stressed by immediate (2 min) and 24-h exposure to the five stress-inducing compounds were monitored by pulse amplitude modulated fluorometry. Cells of Synechocystis sp. PCC 6803 readily survive encapsulation in both alkoxide-derived gels and gels from aqueous precursors and can remain active at least 8 weeks with slight degradation in PSII efficiency. Post-encapsulation survival was improved in gels containing no additive when compared with gels containing PEG or glycerol. Glycerol was shown to have a detrimental effect on Synechocystis sp. PCC 6803, reducing ϕPSII and F(v)'/F(m)' by as much as 75%, possibly a result of disrupting excitation transfer between the phycobilisomes and photosystems. PEG was similarly deleterious, dramatically reducing the ability to carry out a state transition and adequately manage excitation energy distribution. EtOH stress also hindered state transitions, although less severely than PEG, and the cells were able to recover nearly all photosynthetic efficiency within 24 h after an initial drop. Betaine did not interfere with state transitions but did reduce quantum yield and photochemical quenching. Finally, Synechocystis sp. PCC 6803 was shown to recover from salt stress.

  7. Preparation of TiO2-SiO2 via sol-gel method: Effect of Silica precursor on Catalytic and Photocatalytic properties

    Science.gov (United States)

    Fatimah, I.

    2017-02-01

    TiO2-SiO2have been synthesized by the sol-gel method from titanium isopropoxide and varied silica precursors: tetraethyl orthosilicate and tetra methyl ortho silicate. To study the effect of the precursor, prepared materials were characterized by X-ray diffraction, scanning electron microscopy, Diffuse Reflectance UV-vis optical absorption, and also gas sorption analysis. XRD patterns showed the formation of TiO2 anatase in the TiO2-SiO2 composite with different crystallite size from different silica precursor as well as the different surface morphology. The DRUV-vis absorption spectra exhibit similar band gap energy correspond to 3.21eV value while the surface area, pore volume and pore radius of the materials seems to be affected by the precursor. The higher specific surface area contributes to give the enhanced activity in phenol hydroxylation and methylene blue photodegradation.

  8. Distribution threshold values of CaCl2 onto the 10X-zeolite and macro-pore silica gel

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    The calcium chloride used for adsorption separation of ammonia is promising for its large adsorptive capacity and lower desorption temperature,but difficult to develop because of the liable expansion,lump and chip in the adsorption/desorption process.Composite adsorbents made by monolayer dis-persion of calcium chloride onto carriers with high surface areas exhibit better adsorptive capacity and stability.Several models were developed to confirm the maximum monolayer dispersion capacity of calcium chloride onto the carriers(the distribution threshold value),and the closely packed monolayer dispersion model was considered the most suitable for this study.The distribution threshold values given by this model were 0.60 g CaCl2/(g 10X-zeolite) and 0.38 g CaCl2/(g SiO2).When the divalent salt was dispersed onto the carriers,however,anions were separated into two types,causing that the en-tropy of the system tended to increase and the system was not stable.To minimize the entropy,a new model was put forward as the modified closely packed monolayer dispersion model.Based on this model,the distribution threshold values are 0.52 g CaCl2/(g 10X-zeolite) and 0.33 g CaCl2/(g SiO2),re-spectively.The distribution threshold values were also gained experimentally by XRD quantitative phase analysis:0.61 g CaCl2/(g 10X-zeolite) and 0.31 g CaCl2/(g SiO2).Comparison between experi-mental values of distribution threshold with theoretical ones based on two different model showed that the closely packed monolayer dispersion model fits the monolayer dispersion of calcium chloride onto micro-pore carrier - 10X-zeolite,and the modified closely packed monolayer dispersion model is more suitable for the bigger aperture carrier - macro-pore silica gel.

  9. In Situ Immobilization on the Silica Gel Surface and Adsorption Capacity of Poly[ N-(4-carboxyphenyl)methacrylamide] on Toxic Metal Ions

    Science.gov (United States)

    Yanovska, Elina; Savchenko, Irina; Sternik, Dariusz; Kychkiruk, Olga; Ol'khovik, Lidiya; Buriachenko, Iana

    2017-04-01

    In situ immobilization of poly[ N-(4-carboxyphenyl)methacrylamide] has been performed on silica gel surface. Infrared (IR) and mass spectroscopies as well as thermogravimetry (TG) analysis have been used to elucidate the structure of immobilized polymer. An adsorption capacity of the synthesized composite towards Cu(II), Pb(II), Mn(II), Fe(III), Co(II), and Ni(II) ions has been estimated. Adsorption activity to microquantities of Pb(II), Cu(II), and Ni(II) in a neutral aqueous medium has been observed.

  10. Covalently grafted, silica gel supported C-protected cysteine or cystine copper complexes - syntheses, structure and possible surface reactions studied by FT-IR spectroscopy

    Science.gov (United States)

    Aranyi, A.; Csendes, Z.; Kiss, J. T.; Pálinkó, I.

    2009-04-01

    In this work the covalent anchoring of C-protected Cu(II)- L-cysteine and Cu(II)- L-cystine complexes onto a surface-modified silica gel is described. Conditions of the syntheses were varied and the obtained structures were studied by classical analytical (titration) as well as spectroscopic (infrared, atomic absorption) methods. It was found that the sulphur atoms in the molecules acted as primary coordination sites, while the other coordinating groups varied depending on whether the complexes were formed under ligand-poor or ligand-excess conditions.

  11. Tethered ansa-bridged titanium complexes immobilized on 3-mercaptopropyl-functionalized silica gel and their application for the hydrosilylation of imines.

    Science.gov (United States)

    Gruber-Woelfler, Heidrun; Lichtenegger, Georg J; Neubauer, Christoph; Polo, Eleonora; Khinast, Johannes G

    2012-11-07

    Four tethered titanocene complexes were covalently immobilized onto 3-mercaptopropyl-functionalized silica gel. We have investigated the influence of the length of the tether and of the ansa-bridge on the activity in the heterogeneous hydrosilylation of the cyclic imine 2-phenylpyrroline, taken as an illustrative example. Possible metal leaching during the reaction was investigated using ICP/OES, recycling studies and the three-phase test. The novel immobilized catalysts exhibit an activity similar to their homogeneous analogues in the tested hydrosilylation reactions with a TOF of ~20 h(-1). Furthermore, our results indicate that metal leaching is negligible under the applied reaction conditions.

  12. Al(HSO_4)_3/silica gel as a novel catalytic system for the ring opening of epoxides with thiocyanate anion under solvent-free conditions

    Institute of Scientific and Technical Information of China (English)

    Ali; Reza; Kiasat; Arash; Mouradzadegun; Somayeh; Elahi; Mehdi; Fallah-Mehrjardi

    2010-01-01

    For the first time,metal hydrogen sulfates and phosphates/silica gel have been studied as efficient and powerful solid acid catalysts in the ring opening of epoxides with thiocyanate anion.The most significant result was obtained by Al(HSO_4)_3/SiO_2 which afforded the corresponding β-hydroxy thiocyanates under mild reaction conditions and in very short reaction times.The cheapness, availability of the catalyst,ease of procedure and work-up make this method attractive for the organic synthesis.

  13. Silica-gel-supported Phosphorus Pentoxide: a Simple and Efficient Solid-supported Reagent for Esterification of Long-Chain Carboxylic Acids and Their Antimicrobial Screening

    Institute of Scientific and Technical Information of China (English)

    RAUF Abdul; GANGAL Saloni; SHARMA Shweta

    2008-01-01

    A silica-gel-supported heterogeneous phosphorus pentoxide reagent has been developed for the esterification of various long-chain carboxylic acids with aromatic alcohols. The reactions occurred under relatively mild conditions and afforded the desired products in good yields. All the compounds 3a-3x were screened for antibacterial and antifungal activity, which showed good activity against Gram positive and Gram negative bacteria and also good results against almost all fungal strains. The structures of the synthesized compounds were elucidated by IR, 1H NMR,13C NMR, mass spectroscopic techniques and elemental analysis.

  14. STUDY ON ENRICHMENT AND SEPARATION OF TRACE Pd(Ⅱ) WHITH SILICA GEL BONDED BY (BENZOYLAZO—ARSENAZO I)—AMINOPROPYL

    Institute of Scientific and Technical Information of China (English)

    LIUFeng; LIKean; 等

    1992-01-01

    This Paper reports enrichment and sepqration of trace Pd(Ⅱ)with silica gel bonded by (benzolyazo-arsenazo I)-aminopropyl(BAAI·SG).BAAI·SG is stable in solution between 6 mol/L HCl and pH 9.0.The maximum adsorptive capacities of BAAI·SG and SG are 52.7,23.5μmol/g respectively.After preconcentration through BAII·SG column,Pd(Ⅱ)of ppb level in artificial water samples can be measured by spectrophotometry.

  15. Validation of an RPHPTLC-Densitometric Method Using Silica Gel 60 RP18WF254 for Simultaneous Determination of Nicotinamide in Selected Pharmaceutical Formulations

    OpenAIRE

    Małgorzata Dołowy; Alina Pyka

    2015-01-01

    This research study describes the applicability of silica gel 60 RPW18F254 plates for the development and validation of new, simple, economic, accurate, and precise RPHPTLC-densitometric method suitable for the quantification of nicotinamide (as Vitamin PP) in three marketed preparations. The mobile phase used was methanol-water in volume composition 3 : 7. Detection wavelength was 200 nm. The proposed method was validated according to ICH guidelines and also based on Ferenczi-Fodor and Konie...

  16. Effect of the size of silica nanoparticles on wettability and surface chemistry of sol–gel superhydrophobic and oleophobic nanocomposite coatings

    Energy Technology Data Exchange (ETDEWEB)

    Lakshmi, R.V., E-mail: lakshmi_rv@nal.res.in; Bera, Parthasarathi; Anandan, C.; Basu, Bharathibai J.

    2014-11-30

    Highlights: • Superhydrophobic coatings from Cab-O-Sil EH5 and M5 particles in MTEOS sol. • Particle size of Cab-O-Sil influenced its optimum concentration in coating. • FAS-13 modification improved the oleophobicity of the coating. • Coating surface exhibited porous structure with nanovoids and microscale bumps. • Coatings with Cab-O-Sil EH5 retained water repelling property for a long time. - Abstract: Superhydrophobic sol–gel nanocomposite coatings have been fabricated by incorporating silica nanoparticles with different particle sizes separately in an acid-catalyzed sol of methyltriethoxysilane (MTEOS). Water contact angle (WCA) of the coatings increased with increase in the concentration of silica nanoparticles in both the cases. The coatings became superhydrophobic at an optimum silica concentration. The water repellency was further improved by the addition of fluoroalkylsilane (FAS). The optimum silica concentration was found to depend on the size of silica nanoparticles and FAS content and the coatings exhibited WCA of about 160° and water sliding angle (WSA) of <2°. FAS addition also improved the oleophobicity of the coatings. The coatings exhibited oil-repellency with a lubricant oil contact angle of 126° and ethylene glycol contact angle of 153.3°. Surface morphology of the coatings analyzed using field emission scanning electron microscopy (FESEM) showed a rough surface with microscale bumps and nanoscale pores. XPS was used to study the surface composition of the coatings. The superhydrophobic property of the coatings was due to the synergistic effect of surface chemistry and surface microstructure and can be explained using Cassie-Baxter model.

  17. The solid phase extraction of some metal ions using palladium nanoparticles attached to silica gel chemically bonded by silica-bonded N-propylmorpholine as new sorbent prior to their determination by flame atomic absorption spectroscopy.

    Science.gov (United States)

    Ghaedi, M; Rezakhani, M; Khodadoust, S; Niknam, K; Soylak, M

    2012-01-01

    In this research at first palladium nanoparticle attached to a new chemically bonded silica gel has been synthesized and has been characterized with different techniques such as X-ray diffraction (XRD), fourier transform infrared (FT-IR), transmission electron microscopy (TEM), and scanning electron microscopy (SEM). Then, this new sorbent (chemically modified silica gel with N-propylmorpholine (PNP-SBNPM)) was efficiently used for preconcentration of some metal ions in various food samples. The influence of effective variables including mass of sorbent, flow rate, pH of sample solutions and condition of eluent such as volume, type and concentration on the recoveries of understudy metal ions were investigated. Following the optimization of variables, the interfering effects of some foreign ions on the preconcentration and determination of the investigated metal ions described. At optimum values of variables, all investigated metal ions were efficiently recovered with efficiency more than 95%, relative standard deviation (RSD) between 2.4 and 2.8, and detection limit in the range of 1.4-2.7 ng mL⁻¹. The present method is simple and rapidly applicable for the determination of the understudied metal ions (ng mL⁻¹) in different natural food samples.

  18. The Solid Phase Extraction of Some Metal Ions Using Palladium Nanoparticles Attached to Silica Gel Chemically Bonded by Silica-Bonded N-Propylmorpholine as New Sorbent prior to Their Determination by Flame Atomic Absorption Spectroscopy

    Directory of Open Access Journals (Sweden)

    M. Ghaedi

    2012-01-01

    Full Text Available In this research at first palladium nanoparticle attached to a new chemically bonded silica gel has been synthesized and has been characterized with different techniques such as X-ray diffraction (XRD, fourier transform infrared (FT-IR, transmission electron microscopy (TEM, and scanning electron microscopy (SEM. Then, this new sorbent (chemically modified silica gel with N-propylmorpholine (PNP-SBNPM was efficiently used for preconcentration of some metal ions in various food samples. The influence of effective variables including mass of sorbent, flow rate, pH of sample solutions and condition of eluent such as volume, type and concentration on the recoveries of understudy metal ions were investigated. Following the optimization of variables, the interfering effects of some foreign ions on the preconcentration and determination of the investigated metal ions described. At optimum values of variables, all investigated metal ions were efficiently recovered with efficiency more than 95%, relative standard deviation (RSD between 2.4 and 2.8, and detection limit in the range of 1.4–2.7 ng mL−1. The present method is simple and rapidly applicable for the determination of the understudied metal ions (ng mL−1 in different natural food samples.

  19. Improvement of Mechanical, Thermal and Optical Properties of Barium Mixed Cobalt Tartrate Hydrate Crystals Grown by Gel Method

    OpenAIRE

    2015-01-01

    In this present work, CTH and BCTH crystals have been prepared by gel technique by using single diffusion method at room temperature. The as grown crystals were characterized by using XRD, FT-IR, UV, TG / DTA and Micro hardness studies. X-ray powder diffraction results analyzed by using suitable software suggest that a CTH and BCTH crystals belong to cubic crystal system. The unit cell volume is observed to increase with increase in the concentration of barium in cobalt tartrate due to the la...

  20. Preconcentration of lead, cadmium and zinc on silica gel loaded with diethyldithiocarbamate prior to their determination by flame-atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Rio-Segade, S. [Dept. de Quimica Analitica y Alimentaria, Univ. de Vigo, Orense (Spain); Perez-Cid, B. [Dept. de Quimica Analitica y Alimentaria, Univ. de Vigo, Orense (Spain); Bendicho, C. [Dept. de Quimica Analitica y Alimentaria, Univ. de Vigo, Orense (Spain)

    1995-04-01

    A silica gel sorbent loaded with sodium diethyldithiocarbamate has been developed for the preconcentration of lead, cadmium and zinc prior to their determination by flame-atomic absorption spectrometry (FAAS). The sorption and desorption of the metal ions was studied under both static and dynamic conditions. The metal ions were quantitatively retained on the silica gel sorbent based on an equilibrium time of less than 1 min. In case of the batch method, the effects of pH, shaking time, amount of sorbent, and desorption time were investigated. Among the desorption agents studied, only EDTA in ammonium chloride/ammonia buffer yielded quantitative recoveries. Freundlich`s sorption isotherms determined for each metal show that sufficient sorption ability is obtained. The column method allows the preconcentration of metal ions from large sample volumes (e.g. 200 mL) using a flow rate of 5 mL min{sup -1}. The influence of foreign ions present in natural waters and saline solutions was examined. The reproducibility of the total analytical method, expressed as relative standard deviation (RSD) is 1.8, 0.5 and 0.6%, for lead, cadmium and zinc, respectively. (orig.)

  1. Silica-gel Particles Loaded with an Ionic Liquid for Separation of Zr(IV Prior to Its Determination by ICP-OES

    Directory of Open Access Journals (Sweden)

    Hadi M. Marwani

    2016-06-01

    Full Text Available A new ionic liquid loaded silica gel amine (SG-APTMS-N,N-EPANTf2 was developed, as an adsorptive material, for selective adsorption and determination of zirconium, Zr(IV, without the need for a chelating intermediate. Based on a selectivity study, the SG-APTMS-N,N-EPANTf2 phase showed a perfect selectivity towards Zr(IV at pH 4 as compared to other metallic ions, including gold [Au(III], copper [Cu(II], cobalt [Co(II], chromium [Cr(III], lead [Pb(II], selenium [Se(IV] and mercury [Hg(II] ions. The influence of pH, Zr(IV concentration, contact time and interfering ions on SG-APTMS-N,N-EPANTf2 uptake for Zr(IV was evaluated. The presence of incorporated donor atoms in newly synthesized SG-APTMS-N,N-EPANTf2 phase played a significant role in enhancing its uptake capacity of Zr(IV by 78.64% in contrast to silica gel (activated. The equilibrium and kinetic information of Zr(IV adsorption onto SG-APTMS-N,N-EPANTf2 were best expressed by Langmuir and pseudo second-order kinetic models, respectively. General co-existing cations did not interfere with the extraction and detection of Zr(IV. Finally, the analytical efficiency of the newly developed method was also confirmed by implementing it for the determination of Zr(IV in several water samples.

  2. Performance Evaluation of a Continuous Operation Adsorption Chiller Powered by Solar Energy Using Silica Gel and Water as the Working Pair

    Directory of Open Access Journals (Sweden)

    Hassan Zohair Hassan

    2014-10-01

    Full Text Available In the present study, dynamic analysis and performance evaluation of a solar-powered continuous operation adsorption chiller are introduced. The adsorption chiller uses silica gel and water as the working pair. The developed mathematical model represents the heat and mass transfer within the reactor coupled with the energy balance of the collector plate and the glass cover. Moreover, a non-equilibrium adsorption kinetic model is taken into account by using the linear driving force equation. The variation of solar radiation, wind speed, and atmospheric temperature along a complete cycle are considered for a more realistic simulation. Based on the case studied  and the baseline parameters, the chiller is found to acquire a coefficient of performance of 0.402. The average thermal efficiency of the solar collector is estimated to be 62.96% and the average total efficiency  approaches a value of 50.91%. Other performance parameters obtained are 363.8 W and 1.82 W/kg for the cooling capacity and the specific cooling power of the chiller, respectively. Furthermore, every 1 kg of silica gel inside the adsorption reactor produces a daily chilled water mass of 3 kg at a temperature of 10 ◦C. In addition, the cooling system harnesses 25.35% of the total available solar radiation and converts it to a cooling effect.

  3. Effect of the silanization conditions on chromatographic behavior of an open-tubular capillary column coated with a modified silica-gel thin layer.

    Science.gov (United States)

    Nakano, Yusuke; Kitagawa, Shinya; Miyabe, Kanji; Tsuda, Takao

    2005-10-01

    The performance of an open-tubular capillary column coated with a modified silica-gel thin layer was investigated, particularly concerning the effect of the silanization process on it. Although the increase in the octadecyltriethoxysilane (ODTES) concentration in the silanization process could enhance the retention factor of naphthalene, its theoretical plate number was significantly reduced (ODTES, 5 to 50%; k, 0.2 to 4.3; N, 79600 to 2600 m(-1)). Namely, the increase in the retention factor was accompanied by a decrease in the theoretical plate number. A similar phenomenon was also observed when octadecyldimethylchlorosilane (ODCS) was used as the silanization regent. However, increases in both the retention factor and the theoretical plate number could be achieved (sample, naphthalene; k, 0.05 to 0.09; N, 149000 to 220000 m(-1)) by a NaOH treatment to the fabricated thin porous silica-gel layer before silanization with ODCS. The electrochromatographic separation of proteins and peptides by using the NaOH-treated column could obtain more peaks than electrophoretic separation.

  4. COVALENTLY BONDING CHIRAL POLYURETHANE ON AMINATED SILICA GEL: A NEW STRATEGY TO PREPARE CHIRAL STATIONARY PHASE FOR HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

    Institute of Scientific and Technical Information of China (English)

    Shao-hua Huang; Zheng-wu Bai; Chuan-qi Yin; Shi-rong Li

    2006-01-01

    Two polyurethanes of different molecular weights were prepared by the copolymerization of phenyl diisocyanate and diisopropyl tartrate. The polyurethanes having terminal isocyanate groups were reacted with 3-aminopropyl silica gel to afford two chiral stationary phases. The (M-)n of the two polyurethanes were 4057 g/mol and 6442 g/mol. The polyurethanes and the corresponding chiral stationary phases were characterized by FT-IR, 1H NMR and elemental analysis. The loading capacities of the polyurethanes on silica gel were 0.68 mmol units/g and 0.61 mmol units/g, respectively. The separation performance and the influence of additives, triethylamine and trichloroacetic acid, on the separation of chiral compounds were investigated by HPLC. The chiral stationary phase prepared from polyurethane with (M-)n of 4057 g/mol demonstrated better enantioseparation capability than that with (M-)n of 6442 g/mol. Additionally, it was found that the addition of triethylamine and trichloroacetic acid in the mobile phases significantly improved the enantioseparation for these two chiral stationary phases.

  5. Synthesis and properties of a newly obtained sorbent based on silica gel coated with a polyaniline film as the stationary phase for non-suppressed ion chromatography.

    Science.gov (United States)

    Sowa, Ireneusz; Wójciak-Kosior, Magdalena; Drączkowski, Piotr; Strzemski, Maciej; Kocjan, Ryszard

    2013-07-17

    The new sorbent for non-suppressed ion chromatography based on silica gel coated with a film of polyaniline (PANI) was obtained in a process of in situ polymerization of aniline by oxidation with ammonium peroxydisulfate. Raman analyses performed using a Thermo Scientific DXR confocal Raman Microscope equipped with the Omnic 8 software from Thermo Fisher Scientific have proved a uniform distribution of PANI on the surface of chromatographic beads and in the pores of the particle. The obtained stationary phase was packed into a stainless steel HPLC column. The quality of the prepared column was verified on the basis of hydrodynamic parameters such as column efficiency index (Ip) and separation impedance (E). The potential application of silica gel modified with polyaniline for separation and determination of selected anions using non-suppressed ion chromatography was also investigated. Chromatographic analyses were performed using of the ion chromatograph Dionex DX-500. The best results were obtained for the mobile phase consisting of an aqueous or methanolic solution of hydrochloric acid. The tested column and optimized chromatographic system were successfully used for the analysis of nitrate, bromide and iodide in waters samples.

  6. Spectrophotometric Determination of Iron(II after Solid Phase Extraction of Its 2,2′ Bipyridine Complex on Silica Gel-Polyethylene Glycol

    Directory of Open Access Journals (Sweden)

    Nahid Pourreza

    2013-01-01

    Full Text Available A new solid phase extraction procedure was developed for preconcentration of iron(II using silica gel-polyethylene glycol (silica-PEG as an adsorbent. The method is based on retention of iron(II as 2,2′ bipyridine complex on silica-PEG. The retained complex is eluted by 1.0 mol L−1 of sulfuric acid-acetone mixture (1:2 and its absorbance is measured at 518 nm, spectrophotometrically. The effects of different parameters such as pH, concentration of the reagent, eluting reagent, sample volume, amount of adsorbent, and interfering ions were investigated. The calibration graph was linear in the range of 1–60 ng mL−1 of iron(II. The limit of detection based on 3Sb was 0.57 ng mL−1 and relative standard deviations (R.S.D for ten replicate measurements of 12 and 42 ng mL−1 of iron(II were 2.4 and 1.7%, respectively. The method was applied to the determination of of iron(II in water, multivitamin tablet, and spinach samples.

  7. Sol-gel encapsulation of binary Zn(II) compounds in silica nanoparticles. Structure-activity correlations in hybrid materials targeting Zn(II) antibacterial use.

    Science.gov (United States)

    Halevas, E; Nday, C M; Kaprara, E; Psycharis, V; Raptopoulou, C P; Jackson, G E; Litsardakis, G; Salifoglou, A

    2015-10-01

    In the emerging issue of enhanced multi-resistant properties in infectious pathogens, new nanomaterials with optimally efficient antibacterial activity and lower toxicity than other species attract considerable research interest. In an effort to develop such efficient antibacterials, we a) synthesized acid-catalyzed silica-gel matrices, b) evaluated the suitability of these matrices as potential carrier materials for controlled release of ZnSO4 and a new Zn(II) binary complex with a suitably designed well-defined Schiff base, and c) investigated structural and textural properties of the nanomaterials. Physicochemical characterization of the (empty-loaded) silica-nanoparticles led to an optimized material configuration linked to the delivery of the encapsulated antibacterial zinc load. Entrapment and drug release studies showed the competence of hybrid nanoparticles with respect to the a) zinc loading capacity, b) congruence with zinc physicochemical attributes, and c) release profile of their zinc load. The material antimicrobial properties were demonstrated against Gram-positive (Staphylococcus aureus, Bacillus subtilis, Bacillus cereus) and negative (Escherichia coli, Pseudomonas aeruginosa, Xanthomonas campestris) bacteria using modified agar diffusion methods. ZnSO4 showed less extensive antimicrobial behavior compared to Zn(II)-Schiff, implying that the Zn(II)-bound ligand enhances zinc antimicrobial properties. All zinc-loaded nanoparticles were less antimicrobially active than zinc compounds alone, as encapsulation controls their release, thereby attenuating their antimicrobial activity. To this end, as the amount of loaded zinc increases, the antimicrobial behavior of the nano-agent improves. Collectively, for the first time, sol-gel zinc-loaded silica-nanoparticles were shown to exhibit well-defined antimicrobial activity, justifying due attention to further development of antibacterial nanotechnology.

  8. Opinion of the Scientific Committee on Consumer Safety (SCCS) - Revision of the opinion on the safety of the use of Silica, Hydrated Silica, and Silica Surface Modified with Alkyl Silylates (nano form) in cosmetic products.

    Science.gov (United States)

    Sccs; Hoet, P H M

    2016-02-01

    The SCCS has concluded that the evidence, both provided in the submission and that available in scientific literature, is inadequate and insufficient to allow drawing any firm conclusion either for or against the safety of any of the individual SAS material, or any of the SAS categories that are intended for use in cosmetic products. As the SCCS has not been able to conclude on the safety of the synthetic amorphous silica (SAS) materials included in the current submission, the Applicant is advised to follow the SCCS Guidance on Risk Assessment of Nanomaterials (SCCS/1484/12). A brief summary is provided to enable/facilitate future evaluation of the SAS materials in cosmetic products. Copyright © 2015. Published by Elsevier Inc.

  9. Optical properties of silica sol-gel materials singly-and doubly-doped with Eu3+and Gd3+ions

    Institute of Scientific and Technical Information of China (English)

    Natalia Pawlik; Barbara Szpikowska-Sroka; Marta Sołtys; Wojciech A.Pisarski

    2016-01-01

    In present work, the optical and structural properties of silica sol-gel glasses and glass-ceramic materials singly-and dou-bly-doped with Eu3+and Gd3+ions were investigated. The optical properties of studied systems were determined based on absorption, excitation and emission spectra as well as luminescence decay analysis. Conducted studies clearly indicated a significant enhance-ment of visible emission originated from Eu3+ions as a result of changing the excitation mechanism, via Gd3+→Eu3+energy transfer. The luminescence intensity R-ratio was analyzed before and after heat-treatment process upon excitation atλex=393 nm andλex=273 nm. Moreover, the influence of excitation wavelength on luminescence decay time of the 5D0 excited state was also analyzed. The Gd3+→Eu3+energy transfer efficiencies for precursor and annealed samples were calculated based on luminescence lifetime of the 6P7/2 level of Gd3+ions. The X-ray diffraction measurements were conducted to verify the nature of obtained sol-gel materials. In re-sult, the formation of orthorhombic GdF3 nanocrystal phase dispersed in amorphous silica glass host was identified after annealing. Obtained results clearly indicated an incorporation of Eu3+ activators into formed GdF3 nanocrystals. Thus, conducted heat-treatment process led to considerable changes in surrounding environment around Eu3+ions. Actually, it was found that en-ergy transfer phenomenon and heat-treatment process were responsible for significant improvement of Eu3+luminescence in stud-ied sol-gel samples.

  10. Preparation of Silica Gel Immunoaffinity Column for Chloramphenicol Determination%硅胶载体氯霉素免疫亲和柱的制备

    Institute of Scientific and Technical Information of China (English)

    张灿; 周婷; 陆介宇; 段玉清; 王硕; 于娇

    2012-01-01

    以硅胶为载体,通过硅烷偶联剂3-氨基丙基三乙氧基硅烷在其表面引入氨基,采用戊二醛法与氯霉素抗体进行偶联。该方法制备的免疫亲和柱对氯霉素抗体的偶联率达到72%,对氯霉素的最大吸附容量达到80ng/mL柱体积,选择含70%甲醇的PBS为洗脱溶液。以牛奶为检测对象分别采用3种不同方法进行样品处理,利用免疫亲和柱实现对样品中痕量残留的氯霉素纯化富集并进行ELISA检测。%Silica gel was used as a carrier for preparing an immunoaffinity column (IAC) to determine chloramphenicol. Amino groups were introduced to the surface of silica gel using 3-aminopropyltriethoxysilane (APTES) as a silane coupling agent and the modified silica gel was conjugated with anti-chloramphenicol antibodies using glutaraldehyde. As a result, a conjugation ratio of 72% was obtained. The maximum adsorption capacity of the prepared IAC was 80 ng/mL. The elution solvent was PBS containing 70% methanol. After sample pretreatment by three different methods, chloramphenicol residues in milk were ourified and enriched using the IAC and determined by ELISA

  11. Encapsulation of biomolecules for bioanalytical purposes: Preparation of diclofenac antibody-doped nanometer-sized silica particles by reverse micelle and sol-gel processing

    Energy Technology Data Exchange (ETDEWEB)

    Tsagkogeorgas, Fotios [Laboratory of Inorganic and Analytical Chemistry, School of Chemical Engineering, National Technical University of Athens, Iroon Polytechniou 9, 157 73 Athens (Greece); Institute of Hydrochemistry, Technical University of Munich, Marchioninistrasse 17, D-81377 Munich (Germany); Ochsenkuehn-Petropoulou, Maria [Laboratory of Inorganic and Analytical Chemistry, School of Chemical Engineering, National Technical University of Athens, Iroon Polytechniou 9, 157 73 Athens (Greece); Niessner, Reinhard [Institute of Hydrochemistry, Technical University of Munich, Marchioninistrasse 17, D-81377 Munich (Germany); Knopp, Dietmar [Institute of Hydrochemistry, Technical University of Munich, Marchioninistrasse 17, D-81377 Munich (Germany)]. E-mail: dietmar.knopp@ch.tum.de

    2006-07-28

    In recent years, the sol-gel technique has attracted increasing interest as a unique approach to immobilize biomolecules for bioanalytical applications as well as biochemical and biophysical studies. For this purpose, crushed biomolecule-doped sol-gel glass monoliths have been widely used. In the present work, for the first time, the encapsulation of anti-diclofenac antibodies in silica nanoparticles was carried out by a combination of reverse micelle and sol-gel technique. Cyclohexane was used for the preparation of the microemulsion as organic solvent, while surfactant Igepal CO-520 was found to be the optimal stabilizer. The antibody source was a purified IgG fraction originating from a polyclonal rabbit antiserum. Tetramethyl orthosilicate (TMOS) was used as precursor. Rather uniform, monodispersed and spherical silica particles of about 70 nm diameter size were fabricated, as was demonstrated by transmission electron microscopy (TEM) and scanning electron microscopy/energy dispersive X-ray fluorescence analysis (SEM/EDX). The biological activity of the encapsulated antibodies was evaluated by incubation of the nanoparticles with a diclofenac standard solution and analysis of the filtrate and followed washing solutions by a highly sensitive enzyme-linked immunosorbent assay (ELISA), using non-doped particles as blanks. While only about 6% of the added diclofenac was nonspecifically retained by the blank, the corresponding amount of about 66% was much higher with the antibody-doped particles. An obvious advantage of this approach is the general applicability of the developed technique for a mild immobilization of different antibody species.

  12. Bedded jaspers of the Ordovician Løkken ophiolite, Norway: seafloor deposition and diagenetic maturation of hydrothermal plume-derived silica-iron gels

    Science.gov (United States)

    Grenne, Tor; Slack, John F.

    2003-01-01

    Sedimentary beds of jasper (red hematitic chert) in the Ordovician Løkken ophiolite of Norway are closely associated with volcanogenic massive sulphide (VMS) deposits. The jaspers occur in the immediate hangingwall and laterally peripheral to the large Løkken (25–30 Mt) and small Høydal (0.1 Mt) VMS deposits, and are exposed discontinuously for several kilometres along strike. Massive or laminated types predominate; jasper-sulphide debris-flow deposits are also abundant near VMS deposits. The jaspers contain hematite-rich laminae showing soft-sediment deformation structures and microtextural evidence that record the presence of a colloidal precursor and an origin as gels. Early textures include: (1) straight or curved chains of hematitic filaments 3–10 µm in diameter and 20–100 µm long; (2) branching networks of 15–25 µm-thick, tubular structures surrounded by cryptocrystalline hematite and filled with quartz and euhedral hematite; (3) small (up to 10 µm) spherules composed of cryptocrystalline hematite and silica; and (4) up to 50 µm silica spherules with hematitic cores. The small filaments seem to have been deposited in varying proportions in the primary laminae, possibly together with hematitic and siliceous microspheroids. Diagenetic changes are represented by polygonal syneresis cracks, and the presence of cryptocrystalline (originally opaline) silica, chalcedony, quartz, carbonate and cryptocrystalline hematite and/or goethite forming botryoidal masses and spheroids <10 µm to 5 mm in diameter. Coarser euhedral grains of quartz, carbonate, and hematite are integral parts of these textures. Bleached, silica-rich jaspers preserve only small relics of fine-grained hematite-rich domains, and locally contain sparse pockets composed of coarse euhedral hematite±epidote.

  13. Structural aspects and porosity features of nano-size high surface area alumina-silica mixed oxide catalyst generated through hybrid sol-gel route

    Energy Technology Data Exchange (ETDEWEB)

    Padmaja, P. [Ceramic Technology Division, Regional Research Laboratory (CSIR), Trivandrum 695019, Kerala (India)]. E-mail: padmavasudev@yahoo.com; Warrier, K.G.K. [Ceramic Technology Division, Regional Research Laboratory (CSIR), Trivandrum 695019, Kerala (India)]. E-mail: kgk_warrier@yahoo.com; Padmanabhan, M. [School of Chemical Sciences, Mahatma Gandhi University, Kottayam 686560, Kerala (India); Wunderlich, W. [Graduate School of Engineering, Nagoya Institute of Technology, 466-8555 Nagoya (Japan); Berry, F.J. [Department of Chemistry, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom); Mortimer, M. [Department of Chemistry, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom); Creamer, N.J. [Department of Chemistry, Open University, Walton Hall, Milton Keynes MK7 6AA (United Kingdom)

    2006-01-10

    Alumina-silica mixed oxide nano-catalyst materials with compositions 83.6 wt.% Al{sub 2}O{sub 3}-16.4 wt.% SiO{sub 2} (3Al{sub 2}O{sub 3}.1SiO{sub 2}), 71.82 wt.% Al{sub 2}O{sub 3}-28.18 wt.% SiO{sub 2} (3Al{sub 2}O{sub 3}.2SiO{sub 2}), 62.84 wt.% Al{sub 2}O{sub 3}-37.16 wt.% SiO{sub 2} (3Al{sub 2}O{sub 3}.3SiO{sub 2}) and 56.03 wt.% Al{sub 2}O{sub 3}-43.97 wt.% SiO{sub 2} (3Al{sub 2}O{sub 3}.4SiO{sub 2}) have been prepared by a hybrid sol-gel technique using boehmite as the precursor for alumina and tetraethoxysilane as that for silica. The bonding characteristics and coordination features around Al and Si in the mixed oxide catalysts have been studied using FTIR and {sup 27}Al MAS NMR after calcination at 400 deg. C which is the temperature region where cross-condensation is seen to take place. A high BET specific surface area of 287 m{sup 2} g{sup -1} is obtained for 3Al{sub 2}O{sub 3}.1SiO{sub 2} mixed oxide composition. The porosity features are further established by BET adsorption isotherms and pore size distribution analysis. The temperature-programmed desorption studies showed more surface active sites for the silica-rich composition, suggesting enhanced catalytic potential. The TEM features of the mixed oxides showed a homogeneous distribution of alumina and silica phases with particle sizes in the nano-range. The low silica-containing mixed oxide showed a needle-like morphology with a high aspect ratio of 1:50 and {approx}10 nm particle size while the silica-rich composition had particle size in a wide range ({approx}20-75 nm)

  14. Injectable silica-permanganate gel as a slow-release MnO4(-) source for groundwater remediation: rheological properties and release dynamics.

    Science.gov (United States)

    Yang, S; Oostrom, M; Truex, M J; Li, G; Zhong, L

    2016-02-01

    Injectable slow-release permanganate gels (ISRPGs), formed by mixing aqueous KMnO4 solution with fumed silica powders, may have potential applications in remediating chlorinated solvent plumes in groundwater. A series of batch, column, and two-dimensional (2-D) flow cell experiments has been completed to characterize the ISRPG and study the release of permanganate (MnO4(-)) under a variety of conditions. The experiments have provided information on ISRPG rheology, MnO4(-) release dynamics and distribution in porous media, and trichloroethene (TCE) destruction by the ISRPG-released oxidant. The gel possesses shear thinning characteristics, resulting in a relatively low viscosity during mixing, and facilitating subsurface injection and distribution. Batch tests clearly showed that MnO4(-) diffused out from the ISRPG into water. During this process, the gel did not dissolve or disperse into water, but rather maintained its initial shape. Column experiments demonstrated that MnO4(-) release from the ISRPG lasted considerably longer than that from an aqueous solution. In addition, due to the longer release duration, TCE destruction by ISRPG-released MnO4(-) was considerably more effective than that when MnO4(-) was delivered using aqueous solution injection. In the 2-D flow cell experiments, it was demonstrated that ISRPGs released a long-lasting, low-concentration MnO4(-) plume potentially sufficient for sustainable remediation in aquifers.

  15. Improvement of Mechanical, Thermal and Optical Properties of Barium Mixed Cobalt Tartrate Hydrate Crystals Grown by Gel Method

    Directory of Open Access Journals (Sweden)

    S. Vanaja

    2015-10-01

    Full Text Available In this present work, CTH and BCTH crystals have been prepared by gel technique by using single diffusion method at room temperature. The as grown crystals were characterized by using XRD, FT-IR, UV, TG / DTA and Micro hardness studies. X-ray powder diffraction results analyzed by using suitable software suggest that a CTH and BCTH crystals belong to cubic crystal system. The unit cell volume is observed to increase with increase in the concentration of barium in cobalt tartrate due to the lattice distortion. The band gap and optical properties have analyzed by UV-Visible spectrum. The functional groups and compound formation of the crystals have been studied by FT-IR spectrum. The mechanical properties of the grown crystals were tested by using Vicker’s microhardness studies. The work hardening coefficient (n was determined to be 3.7 for CTH, 5.3 for BCTH (1 : 1 and 6.4 for BCTH (2 : 1 and the stiffness constants for different loads were calculated and reported. Thermal analysis suggests that pure cobalt tartrate starts decomposing at 73.2 °C whereas the barium mixed cobalt tartrate brings about better thermal stability which increases with an increase in barium concentration.

  16. Effects of capsid-modified oncolytic adenoviruses and their combinations with gemcitabine or silica gel on pancreatic cancer.

    Science.gov (United States)

    Kangasniemi, Lotta; Parviainen, Suvi; Pisto, Tommi; Koskinen, Mika; Jokinen, Mika; Kiviluoto, Tuula; Cerullo, Vincenzo; Jalonen, Harry; Koski, Anniina; Kangasniemi, Anna; Kanerva, Anna; Pesonen, Sari; Hemminki, Akseli

    2012-07-01

    Conventional cancer treatments often have little impact on the course of advanced pancreatic cancer. Although cancer gene therapy with adenoviruses is a promising developmental approach, the primary receptor is poorly expressed in pancreatic cancers which might compromise efficacy and thus targeting to other receptors could be beneficial. Extended stealth delivery, combination with standard chemotherapy or circumvention of host antiadenoviral immune response might improve efficacy further. In this work, capsid-modified adenoviruses were studied for transduction of cell lines and clinical normal and tumor tissue samples. The respective oncolytic viruses were tested for oncolytic activity in vitro and in vivo. Survival was studied in a peritoneally disseminated pancreas cancer model, with or without concurrent gemcitabine while silica implants were utilized for extended intraperitoneal virus delivery. Immunocompetent mice and Syrian hamsters were used to study the effect of silica mediated delivery on antiviral immune responses and subsequent in vivo gene delivery. Capsid modifications selectively enhanced gene transfer to malignant pancreatic cancer cell lines and clinical samples. The respective oncolytic viruses resulted in increased cell killing in vitro, which translated into a survival benefit in mice. Early proinfammatory cytokine responses and formation of antiviral neutralizing antibodies was partially avoided with silica implants. The implant also shielded the virus from pre-existing neutralizing antibodies, while increasing the pancreas/liver gene delivery ratio six-fold. In conclusion, capsid modified adenoviruses would be useful for testing in pancreatic cancer trials. Silica implants might increase the safety and efficacy of the approach.

  17. PVDF-HFP/silica-SH nanocomposite synthesis for PEMFC membranes through simultaneous one-step sol–gel reaction and reactive extrusion

    Energy Technology Data Exchange (ETDEWEB)

    Seck, S. [Université de Lyon, Université Lyon 1, UMR CNRS 5223 Ingénierie des Matériaux Polymères, IMP@Lyon1, Bât PolyTech, 15 Boulevard Latarjet, 69622 Villeurbanne Cedex (France); Université de Lyon, INSA, UMR CNRS 5223 Ingénierie des Matériaux Polymères IMP@INSA, Batîment Jules Verne, 17 avenue Jean Capelle, 69621 Villeurbanne Cedex (France); Magana, S. [Université de Lyon, Université Lyon 1, UMR CNRS 5223 Ingénierie des Matériaux Polymères, IMP@Lyon1, Bât PolyTech, 15 Boulevard Latarjet, 69622 Villeurbanne Cedex (France); Prébé, A.; Niepceron, F. [Université de Lyon, Université Lyon 1, UMR CNRS 5223 Ingénierie des Matériaux Polymères, IMP@Lyon1, Bât PolyTech, 15 Boulevard Latarjet, 69622 Villeurbanne Cedex (France); Université de Lyon, INSA, UMR CNRS 5223 Ingénierie des Matériaux Polymères IMP@INSA, Batîment Jules Verne, 17 avenue Jean Capelle, 69621 Villeurbanne Cedex (France); and others

    2015-08-01

    In this study, synthesis of thiol-functionalized silica/PVDF-HFP [poly(vinylidene fluoride-hexafluoropropylene)] nanocomposite materials was carried out by reactive extrusion through in situ sol–gel reactions of an alkoxysilane inorganic precursor solution composed of polydimethoxysiloxane (PDMOS) and mercaptopropyltriethoxysilane (MPTES). Successful introduction of the functional MPTES and structural PDMOS alkoxysilanes, and subsequent condensation reactions in the PVDF-HFP, were obtained through pre-hydrolysis reactions of the precursors. {sup 29}Si-Nuclear magnetic resonance was used to assess the hydrolysis level of the inorganic precursor solution and condensation state in the resulting PVDF-HFP/functionalized silica nanocomposites, while the morphology was observed using scanning electron microscopy (SEM). The hydrolysis-condensation reactions resulting in the inorganic phase were optimized by setting an appropriate R{sub 0} molar ratio (H{sub 2}O/alkoxy function), R{sub 1} molar ratio (MPTES/PDMOS) and pH of the solution. Increasing the R{sub 0} ratio barely affected the hydrolysis kinetics. However, a higher R{sub 1} ratio led to a decrease in the inorganic precursors condensation state and consequently to an increase in the reaction time in the extruder to reach the subsequent condensation state. Hence the morphology of the obtained nanocomposites was finer for the highest R{sub 1} ratio and in agreement with the evolution of the solubility parameters. Promising ionic exchange capacity (IEC) and conductivity values were obtained for these innovative nanocomposite materials thanks to a controlled oxidation reaction of the thiol groups into sulfonic acid functions. This original approach demonstrated the possibility of incorporating in situ functionalized silica into a molten fluorinated polymer matrix in a unique reactive extrusion procedure. - Highlights: • Thiol-functionalized silica/PVDF-HFP nanocomposite synthesis by sol–gel and extrusion.

  18. Heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel and its application to a flow analytical system using flame atomic absorption spectrometry

    Energy Technology Data Exchange (ETDEWEB)

    Mori, Masanobu, E-mail: mori@gunma-u.ac.jp [Graduate School of Science and Technology, Gunma University, 1-5-1, Tenjin-cho, Kiryu 376-8515, Japan, (Japan); Suzuki, Toshinobu; Sugita, Tsuyoshi; Nagai, Daisuke [Graduate School of Science and Technology, Gunma University, 1-5-1, Tenjin-cho, Kiryu 376-8515, Japan, (Japan); Hirayama, Kazuo [College of Engineering, Nihon University, 1 Nakagawara, Tokusada, Tamuramachi, Koriyama, Fukushima 963-8642 (Japan); Onozato, Makoto; Itabashi, Hideyuki [Graduate School of Science and Technology, Gunma University, 1-5-1, Tenjin-cho, Kiryu 376-8515, Japan, (Japan)

    2014-08-20

    Highlights: • Calcium-alginate-modified dien-silica gel adsorbed multivalent metal ions. • Metal ions adsorbed on CaAD were eluted using low acidic concentrations. • Flow system with CaAD-packed column enriched metal concentrations up to 50-fold. - Abstract: This study aimed to evaluate the heavy metal adsorptivity of calcium-alginate-modified diethylenetriamine-silica gel (CaAD) and incorporate this biosorbent into a flow analytical system for heavy metal ions using flame atomic absorption spectrometry (FAAS). The biosorbent was synthesized by electrostatically coating calcium alginate onto diethylenetriamine (dien)-silica gel. Copper ion adsorption tests by a batch method showed that CaAD exhibited a higher adsorption rate compared with other biosorbents despite its low maximum adsorption capacity. Next, CaAD was packed into a 1 mL microcolumn, which was connected to a flow analytical system equipped with an FAAS instrument. The flow system quantitatively adsorbed heavy metals and enriched their concentrations. This quantitative adsorption was achieved for pH 3–4 solutions containing 1.0 × 10{sup −6} M of heavy metal ions at a flow rate of 5.0 mL min{sup −1}. Furthermore, the metal ions were successfully desorbed from CaAD at low nitric acid concentrations (0.05–0.15 M) than from the polyaminecarboxylic acid chelating resin (Chelex 100). Therefore, CaAD may be considered as a biosorbent that quickly adsorbs and easily desorbs analyte metal ions. In addition, the flow system enhanced the concentrations of heavy metals such as Cu{sup 2+}, Zn{sup 2+}, and Pb{sup 2+} by 50-fold. This new enrichment system successfully performed the separation and determination of Cu{sup 2+} (5.0 × 10{sup −8} M) and Zn{sup 2+} (5.7 × 10{sup −8} M) in a river water sample and Pb{sup 2+} (3.8 × 10{sup −9} M) in a ground water sample.

  19. High performance thin-layer chromatography-mass spectrometry of Japanese knotweed flavan-3-ols and proanthocyanidins on silica gel plates.

    Science.gov (United States)

    Glavnik, Vesna; Vovk, Irena; Albreht, Alen

    2017-01-27

    On-line elution based TLC-MS is now a well-established technique, but the quality of the data obtained can sometimes be hampered by a severe spectral background or by strong ion suppression, especially when silica gel plates are used in combination with an acidic modifier in the developing solvent. We solved this issue simply and efficiently using two pre-developments of the plates, firstly with methanol-formic acid (10:1, v/v) and secondly with acetonitrile-methanol (2:1, v/v). This solution resulted in significant improvement in the sensitivity of HPTLC-MS methods. The applicability of this approach was proven on analysis of flavan-3-ols and proanthocyanidins in crude extracts of Japanese knotweed (Fallopia japonica Houtt.) rhizomes. Separations on HPTLC silica gel and HPTLC silica gel MS grade plates using developing solvents toluene-acetone-formic acid (3:3:1, 6:6:1, 3:6:1, v/v) and dichloromethane-acetone-formic acid (1:1:0.1, v/v) were followed by post-chromatographic derivatization with 4-dimethylaminocinnamaldehyde (DMACA) detection reagent. Examination of the stability of the analytes on the start confirmed that the plates should be developed immediately after the application of standards and sample test solutions. In a five hours stability testing after development we discovered an unexpected phenomenon of enhanced absorption at 280nm. However, based on an experiment with post-chromatographic derivatization with DMACA detection reagent, the analytes were proven to be sufficiently stable in the time frame of an HPTLC-MS analysis. This was important for development of the first HPTLC-MS and HPTLC-MS(n) methods for identification of flavan-3-ols and B-type proanthocyanidins from monomers up to decamers. For the first time, based on this research methodology, trimers, trimer gallates, tetramer gallates, pentamers, pentamer gallates, hexamers, hexamer gallates, heptamers, octamers, nonamers and decamers were tentatively identified in Japanese knotweed rhizomes

  20. Syntheses, characterization and adsorption properties for Pb{sup 2+} of silica-gel functionalized by dendrimer-like polyamidoamine and 5-sulfosalicylic acid

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Xiongzhi, E-mail: 2004046@glut.edu.cn; Luo, Liangliang; Chen, Ziyan; Liang, Kailing

    2016-02-28

    Graphical abstract: SEM images of APSG, PAMAM-1.0SSASG, PAMAM-2.0SSASG, PAMAM-3.0SSASG and PAMAM-4.0SSASG. - Highlights: • Silica-gel adsorbents PAMAM-n.0SSASG (n = 1–4) with dendrimer-like polyamidoamine and 5-sulfosalicylic acid as functional groups were prepared. • The generation increase of grafted PAMAM changed the pore diameter distribution of adsorbent and adsorption/desorption property of PAMAM-4.0SSASG for Pb{sup 2+} was the best of four adsorbents. • The priority of adsorption property of PAMAM-4.0SSASG was explained by steric hindrance effect of PAMAM on adsorption/desorption, and selective adsorption of 5-sulfosalicylic acid with Pb{sup 2+}. • Pb{sup 2+} in standard reference sample and sea water sample were preconcentrated with PAMAM-4.0SSASG as adsorbent and determined by GFAAS. - Abstract: Silica-gel adsorbents PAMAM-n.0SSASG (n = 1–4) with dendrimer-like polyamidoamine (PAMAM) and 5-sulfosalicylic acid as functional groups were prepared and characterized with FTIR, SEM, TG, elemental analysis and porous structure analysis. Micro-column enrichment and measurement of Pb{sup 2+} with graphite furnace atomic absorption spectroscopy (GFAAS) was studied with PAMAM-n.0SSASG (n = 1–4) as adsorbent. It was emphasized to investigate the relationship between dynamic adsorption/desorption rates, adsorption capacities, and grafting percentage of PAMAM onto silica-gel surface. Experiments showed that the generation increase of grafted PAMAM changed the pore diameter distribution of adsorbent and obviously improved adsorption/desorption property for Pb{sup 2+}. Adsorption capacity of PAMAM-n.0SSASG (n = 1–4) was 14.04, 17.43, 20.07 and 25.05 mg g{sup −1} for Pb{sup 2+} respectively. An enrichment factor of 200 was obtained with PAMAM-4.0SSASG as adsorbent and with 2000 mL Pb{sup 2+} solution (1.0 ng mL{sup −1}). The priority of adsorption property of PAMAM-4.0SSASG was explained by steric hindrance effect of PAMAM on adsorption/desorption, and

  1. Formation of silica iron oxide glasses

    Science.gov (United States)

    Al-Bawab, Abeer F.

    The microemulsion-gel method was developed as an alternative process in the production of room temperature glasses. This method is based on the formation of a microemulsion, to which is added a metal alkoxide that undergoes hydrolysis and condensation to form an oxide network, which is dried into glass. The goal of this work is to understand the sol-gel process upon addition of hydrate metal salts. The thermal transitions of the silica containing ferric nitrate hydrate were examined by differential scanning calorimetry (DSC) and thermal gravimetric analysis (TGA). Using infrared (IR) spectroscopy and X-ray diffraction (XRD). The glasses with a less than 30 mol % iron nitrate were amorphous, while those higher concentration were crystalline. Based on XRD the thermal transitions did not alter the crystallinity. The IR spectra indicated the existence of Si-O-Fe bonds. Thermal analysis indicated similar transitions as exhibited by pure iron nitrate with minor modifications due to interactions with the silica. The reaction between tetraethoxysilane and chloral hydrate in ethanol was followed by NMR of the sp{29}Si nucleus at two different pHs. The sp{29}Si NMR spectra were similar to those reported for the reactions in alcohol between tetraethoxysilane and water of low pH, and for the reactions in the presence of inorganic hydrate. At pH 4, monomene silicon species were detected where at pH 2 the reaction was sufficiently rapid that multi hydroxy monomers were not detected as expected from the catalysts. The reaction proceeded without adding water. The reaction between aluminum chloride and methoxydimethyloctylsilane was investigated at room temperature using NMR and IR spectroscopy in addition to a molecular weight determination from the freezing point reduction in benzene. The structure as deduced from the experimental results was found to be a dimer containing two silicon atoms and two aluminum atoms of which the latter were tetrahedrally coordinated.

  2. Adsorption of simazine on zeolite H-Y and sol-gel technique manufactured porous silica: A comparative study in model and natural waters.

    Science.gov (United States)

    Sannino, Filomena; Marocco, Antonello; Garrone, Edoardo; Esposito, Serena; Pansini, Michele

    2015-01-01

    In this work, we studied the removal of simazine from both a model and well water by adsorption on two different adsorbents: zeolite H-Y and a porous silica made in the laboratory by using the sol-gel technique. The pH dependence of the adsorption process and the isotherms and pseudo-isotherms of adsorption were studied. Moreover, an iterative process of simazine removal from both the model and well water, which allowed us to bring the residual simazine concentration below the maximum concentration (0.05 mg L(-1)) of agrochemicals in wastewater to be released in surface waters or in sink allowed by Italian laws, was proposed. The results obtained were very interesting and the conclusions drawn from them partly differed from what could reasonably be expected.

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

    Science.gov (United States)

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

    2010-01-01

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

  4. An optimized procedure for preconcentration, determination and on-line recovery of palladium using highly selective diphenyldiketone-monothiosemicarbazone modified silica gel.

    Science.gov (United States)

    Sharma, R K; Pandey, Amit; Gulati, Shikha; Adholeya, Alok

    2012-03-30

    A novel, highly selective, efficient and reusable chelating resin, diphenyldiketone-monothiosemicarbazone modified silica gel, was prepared and applied for the on-line separation and preconcentration of Pd(II) ions in catalytic converter and spiked tap water samples. Several parameters like effect of pH, sample volume, flow rate, type of eluent, and influence of various ionic interferences, etc. were evaluated for effective adsorption of palladium at trace levels. The resin was found to be highly selective for Pd(II) ions in the pH range 4-5 with a very high sorption capacity of 0.73 mmol/g and preconcentration factor of 335. The present environment friendly procedure has also been applied for large-scale extraction by employing the use of newly designed reactor in which on-line separation and preconcentration of Pd can be carried out easily and efficiently in short duration of time.

  5. SYNTHESIS OF MESOPOROUS POLY(STYRENE-co-MALEIC ANHYDRIDE)/SILICA HYBRID MATERIALS VIA A NONSURFACTANT-TEMPLATED SOL-GEL PROCESS

    Institute of Scientific and Technical Information of China (English)

    Jie-bin Pang; Kun-yuan Qiu; Yen Wei

    2000-01-01

    Mesoporous poly(styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis was achieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymer in the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template or pore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder Xray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m2/g) and pore volumes (e.g. 0.6 cm3/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, pore volumes and pore diameters of the hybrid materials increase.

  6. Microwave studies on the dielectric properties of Sm{sup 3+} and Sm{sup 3+}/CdTe doped sol-gel silica glasses

    Energy Technology Data Exchange (ETDEWEB)

    Mathew, Siby; Rejikumar, P.R. [School of Pure and Applied Physics, Mahatma Gandhi University, Kottayam 686560 (India); Yohannan, Jaimon; Mathew, K.T. [Department of Electronics, Cochin University of Science and Technology, Cochin 682022 (India); Unnikrishnan, N.V. [School of Pure and Applied Physics, Mahatma Gandhi University, Kottayam 686560 (India)], E-mail: nvu50@yahoo.co.in

    2008-08-25

    Complex permittivity and conductivity studies of Samarium and Samarium/semiconductor cadmium telluride sol-gel silica glass samples were done. We use cavity perturbation technique at S band frequencies using TE{sub 10p} Mode. Structural evolution of the matrix on annealing is discussed based on FTIR analysis/XRD power diffraction. In cavity perturbation technique dielectric parameters like complex permittivity and conductivity are determined by measuring changes in resonant frequency due to small perturbation inside the cavity produced by the introduction of the samples. The addition of the semiconductor along with the samarium was found to lower the permittivity, loss factor and conductivity. Variations of permittivity values with annealing temperature find applications in IC Technology, optic fibre communication, etc. The Sm{sup 3+}/CdTe doped glasses can also be used in the fabrication of new and improved materials for microwave electronic circuits and in electromagnetic shielding devices.

  7. Supported -pyrrolidine-2-carboxylic acid-4-hydrogen sulphate on silica gel as an economical and efficient catalyst for the one-pot preparation of -acetamido ketones via a four-component condensation reaction

    Indian Academy of Sciences (India)

    Arash Ghorbani-Choghamarani; Parisa Zamani

    2014-01-01

    An efficient, one-pot, four-component condensation of aldehydes, acetophenone (or propiophenone), acetyl chloride and acetonitrile in the presence of catalytic amounts of -pyrrolidine-2-carboxylic acid-4-hydrogen sulphate (supported on silica gel), a green and non-toxic catalyst, is described for the preparation of -acetamido ketones in good to excellent yields.

  8. Contribution to the study of the structure and properties of silica gel (1962); Contribution a l'etude de la structure et des proprietes des gels de silice (1962)

    Energy Technology Data Exchange (ETDEWEB)

    Fraissard, J. [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1961-04-15

    The study of the texture of two types of silica gels, xerogels and aerogels, shows that the latter evolve differently on heating. By I.R. spectrography it has been possible to establish that this is due to the existence, in these solids, of a microstructure undetectable by X-rays and which depends on the preparation conditions initially. By using both chemical (thermogravimetry, hydrolysis of diborane) and physical (I.R. spectrography and wide-band N.M.R.) methods we have been able to determine the state of the water of constitution of these gels (water molecules and hydroxyls) and to show that the density, the distribution and the mobility of the protons of this water are very different. For example, the relaxation time T{sub 1} of the protons of a xerogel is about 1 second whilst that of the protons in an aerogel is of the order of a microsecond. Finally, it has been possible by using high resolution N.M.R. to propose a mechanism for the adsorption of formic acid on two types of gel thereby explaining, with the help of previous results, the differences in specificity of these two solids in the decomposition reaction of this acid. (author) [French] L'etude de la texture de deux types de gels de silice, les xerogels et les aerogels, montre que ceux-ci evoluent differemment en fonction de la temperature. La spectrographie I.R a permis de preciser que ceci est du a l'existence, dans ces solides, d'une microstructure indecelable aux rayons X, et fonction des conditions initiales de preparation. Par des methodes chimiques (thermogravimetrie, hydrolyse du diborane) et physiques (spectrographie I.R et R.M.N. large bande), nous avons pu determiner l'etat de l'eau de constitution de ces gels (molecules d'eau et hydroxyles) et montrer que la densite, la repartition et la mobilite des protons de cette eau sont tres differentes. Ainsi le temps de relaxation T{sub 1} des protons d'un xerogel est de l'ordre de la seconde, celui des

  9. Structural and optical properties of Eu3+/Gd3+ ions in silica xerogels and powders obtained by sol-gel method

    Science.gov (United States)

    Pawlik, Natalia; Szpikowska-Sroka, Barbara; Swinarew, Andrzej S.; Łężniak, Marta; Pisarski, Wojciech A.

    2016-12-01

    The xerogels and sol-gel powders with different quantitative composition have been studied based on excitation and emission measurements as well as luminescence decay analysis. The structure of prepared silica sol-gel materials was examined using FT-IR spectroscopy technique. The photoluminescence spectra of Eu3+ ions were registered upon two different excitation wavelengths related to direct excitation of Eu3+ ions (λexc = 393 nm) and indirect excitation through energy transfer process from Gd3+ to Eu3+ (λexc = 273 nm). Upon direct excitation of Eu3+ (7F0 → 5L6 transition) the characteristic emission bands assigned to the 5D0 → 7FJ(0-4) electronic transitions were observed. Also, it was found that enhanced luminescence of Eu3+ is a result of change the excitation parameter through energy transfer phenomenon (8S7/2 → 6IJ transition of Gd3+) and occurred in both xerogels and powder samples. In this way, a UV photon absorbed by Gd3+ is converted into visible light emitted by Eu3+ ions. Obtained results clearly indicated that high concentration of Gd3+ ions in powders led to particularly strong enhance the emission in red spectral range and allowed for more than 12-times prolongation of luminescence lifetime for the 5D0 excited state of Eu3+ compared to silica xerogel samples. The values of energy transfer efficiency were also estimated based on luminescence decay times of the 6P7/2 state of Gd3+ ions.

  10. Isolation and purification of lignans from Schisandra chinensis by combination of silica gel column and high-speed counter-current chromatography

    Directory of Open Access Journals (Sweden)

    Sun Yu

    2013-01-01

    Full Text Available Silica gel column combined with high-speed counter-current chromatography separation was successfully applied to the separation of schizandrin (I, angeloylgomisin H (II, gomisin A (III, schisantherin C (IV, deoxyschizandrin (V, γ-schisandrin (VI and schisandrin C (VII from the fruits of Schisandra chinensis (Turcz. Baillon. The petroleum ether extracts of the fruits of S. chinensis were pre-separated first on a silica gel column and divided into two fractions as sample 1 and sample 2. 260 mg of sample 1 was separated by HSCCC using petroleum ether-ethyl acetate-methanol-water (10:8:10:8, v/v as the two-phase solvent system and 18.2 mg of schizandrin, 15.7 mg of angeloylgomisin H, 16.5 mg of gomisin A and 16.7 mg of schisantherin C were obtained. 230 mg of sample 2 was separated using petroleum ether-ethyl acetate-methanol-water (10:0.5:10:1, v/v as the two-phase solvent system and 19.7 mg of deoxyschizandrin, 23.4 mg of γ-schisandrin and 18.2 mg of schisandrin C were obtained. The purities of the separated compounds were all over 94% as determined by HPLC. The chemical structures of these compounds were confirmed by ESI-MS and 1H NMR. [Acknowledgments. Natural Science Foundation of China (20872083, scientific and technological major special project (2010ZX09401-302-5-12 and the Key Science and Technology Program of Shandong Province (BS2009SW047

  11. A hybrid enrichment process combining conjugated polymer extraction and silica gel adsorption for high purity semiconducting single-walled carbon nanotubes (SWCNT)

    Science.gov (United States)

    Ding, Jianfu; Li, Zhao; Lefebvre, Jacques; Cheng, Fuyong; Dunford, Jeffrey L.; Malenfant, Patrick R. L.; Humes, Jefford; Kroeger, Jens

    2015-09-01

    A novel purification process for the enrichment of sc-SWCNTs that combines selective conjugated polymer extraction (CPE) with selective adsorption using silica gel, termed hybrid-CPE (h-CPE), has been developed, providing a high purity sc-SWCNT material with a significant improvement in process efficiency and yield. Using the h-CPE protocol, a greater than 5 fold improvement in yield can be obtained compared to traditional CPE while obtaining sc-SWCNT with a purity >99.9% as assessed by absorption spectroscopy and Raman mapping. Thin film transistor devices using the h-CPE derived sc-SWCNTs as the semiconductor possess mobility values ranging from 10-30 cm2 V-1 s-1 and current ON/OFF ratio of 104-105 for channel lengths between 2.5 and 20 μm.A novel purification process for the enrichment of sc-SWCNTs that combines selective conjugated polymer extraction (CPE) with selective adsorption using silica gel, termed hybrid-CPE (h-CPE), has been developed, providing a high purity sc-SWCNT material with a significant improvement in process efficiency and yield. Using the h-CPE protocol, a greater than 5 fold improvement in yield can be obtained compared to traditional CPE while obtaining sc-SWCNT with a purity >99.9% as assessed by absorption spectroscopy and Raman mapping. Thin film transistor devices using the h-CPE derived sc-SWCNTs as the semiconductor possess mobility values ranging from 10-30 cm2 V-1 s-1 and current ON/OFF ratio of 104-105 for channel lengths between 2.5 and 20 μm. Electronic supplementary information (ESI) available. See DOI: 10.1039/c5nr04851f

  12. Physicochemical properties of silica gel coated with a thin layer of polyaniline (PANI) and its application in non-suppressed ion chromatography.

    Science.gov (United States)

    Sowa, Ireneusz; Kocjan, Ryszard; Wójciak-Kosior, Magdalena; Swieboda, Ryszard; Zajdel, Dominika; Hajnos, Mieczysław

    2013-10-15

    Physicochemical properties of a new sorbent and its potential application in non-suppressed ion chromatography (IC) have been investigated. The sorbent was obtained in a process of covering silica gel particles with a film of polyaniline (PANI). The properties of silica modified with polyaniline such as particle size, porosity, average quantity of polyaniline covering carrier and density of sorbent were determined. In our study the following methods were used: microscopic analysis, laser diffraction technique, combustion analysis, mercury porosimetry and helium pycnometry. Column with the newly obtained packing was used for the separation of inorganic anions. Optimized chromatographic system was successfully employed for analysis of iodide and bromide in selected pharmaceutical products (Bochnia salt and Iwonicz salt) applied in chronic respiratory disease. Analysis was carried out using 0.1M solution of HCl in mixture of methanol/water (50:50v/v) as a mobile phase; the flow rate was 0.3 mL min(-1), temperature was 24°C and λ=210 nm. Validation parameters such as correlation coefficient, RSD values, recovery, detection and quantification limits were found to be satisfactory. Copyright © 2013 Elsevier B.V. All rights reserved.

  13. Sol–gel processed pyridinium ionic liquid-modified silica as a new sorbent for separation and quantification of iron in water samples

    Directory of Open Access Journals (Sweden)

    H. Abdolmohammad-Zadeh

    2016-09-01

    Full Text Available 1-Hexylpyridinium hexafluorophosphate [C6py][PF6] ionic liquid (IL was firstly used for chemical modification of silica utilizing the acid-catalyzed sol–gel processing. The obtained pyridinium IL-modified silica was employed as a solid phase extraction (SPE sorbent for removal of trace levels of Fe(III ions from aqueous samples. The influence of different variables on the separation efficiency, including the concentration of chelating agent, pH, sample flow rate and volume, eluent type, concentration and volume, and interfering ions was investigated by flame atomic absorption spectrometry (FAAS. In the optimum experimental conditions, the limit of detection (3s, limit of quantification (LOQ and pre-concentration factor were 0.7 μg L−1, 2.5 μg L−1, and 200, respectively. The relative standard deviation (RSD for nine replicate determinations of 25 μg L−1 Fe was 3.2%. The calibration graph using the pre-concentration system was linear in the range of 2.5–50 μg L−1 with a correlation coefficient of 0.9997. The developed method was validated by the analysis of certified reference material and applied successfully to the separation and determination of iron in several water samples.

  14. Triacontyl modified silica gel as a sorbent for the preconcentration of polycyclic aromatic hydrocarbons in aqueous samples prior to gas chromatographic-mass spectrometry determination

    Institute of Scientific and Technical Information of China (English)

    Yan

    2010-01-01

    Triacontyl modified silica gel as a sorbent coupled with gas chromatography-mass spectrometry (GC-MS) was developed to determine EPA prior 16 polycyclic aromatic hydrocarbons (PAHs) in water samples. Various parameters of solid-phase extraction such as organic modifier solvent, eluent, sample flow rate and volume were optimized. The developed method was found to yield a linear calibration curve in the concentration range of 0.05-8 μg/L with respect to naphthalene, acenaphthylene, acenaphthene and 0.01-8μg/L for dibenz[a,h]anthracene and 0.05-14 μg/L for fluorene, phenanthrene, anthracene and 0.01-14 μg/L for the rest of analytes. Furthermore, the good accuracy and repeatability of the method made sure the requirements for achieving reliable analysis of PAHs in the environmental water samples, and the recoveries of optimal method were in the range of 80-120% except to higher volatility PAHs. C30-bonded silica was proved to be an efficient sorbent for extraction of high molecular weight PAHs.

  15. Bifunctional ferromagnetic Eu-Gd-Bi-codoped hybrid organo-silica red emitting phosphors synthesized by a modified Pechini sol-gel method

    Energy Technology Data Exchange (ETDEWEB)

    Abo-Naf, S.M., E-mail: sm.abo-naf@nrc.sci.eg [Glass Research Department, National Research Centre (NRC), El-Buhouth Str., Dokki, 12622 Cairo (Egypt); Abdel-Hameed, S.A.M.; Marzouk, M.A. [Glass Research Department, National Research Centre (NRC), El-Buhouth Str., Dokki, 12622 Cairo (Egypt); Hamdy, Y.M. [Spectroscopy Department, National Research Centre (NRC), El-Buhouth Str., Dokki, 12622 Cairo (Egypt)

    2017-06-15

    Red phosphor, composed of Eu-Gd-Bi-codoped hybrid organo-silica glass, has been synthesized via a modified Pechini sol-gel process. The synthesized hybrid glass was analyzed with powder X-ray diffraction (XRD), differential thermal analysis coupled with thermogravimetry (DTA-TG) and Fourier transform infrared (FTIR) spectroscopy. XRD and DTA-TG confirmed its amorphous structure up to 1000 °C. Magnetic behavior of the produced phosphor was investigated using vibrating specimen magnetometer (VSM) and the obtained results revealed its unsaturated ferromagnetic behavior. Photoluminescence (PL) properties of the obtained phosphor have been investigated under near-UV excitation at 395 nm. The influence of calcination temperature on the PL intensity and its decay behavior as well as on the ferromagnetic characteristics has been studied to determine the optimal reaction temperature of the phosphor. The PL emission spectra show the characteristic emission bands of Eu{sup 3+} ions in the wavelength range from 580 to 700 nm. These emission spectra have been dominated by the electric dipole {sup 5}D{sub 0}→{sup 7}F{sub 2} transition of the Eu{sup 3+} peaked at 610–620 nm producing the red light emission of the phosphors. It was found that the phosphor performance, expressed by its PL intensity and life time, could be significantly improved by increasing of the heat treatment temperature up to 900 °C. Also, calcination at 900 °C for 6 h greatly increased both of the magnetization and retentivity, while decreased the coercivity value. The organic phenomenon of metal citrate-ethylene glycol chelation and its degradation by calcination were well followed by FTIR spectroscopy. The obtained results are promising and could afford a basis for designing of efficient red phosphors for displays, lighting and bifunctional biosensors for biomedical applications. - Highlights: • Eu-Gd-Bi-codoped hybrid organo-silica phosphor was synthesized by sol-gel method. • Inorganic Eu-Gd-Bi-silica

  16. Influência de solventes orgânicos na adsorção de linalol e decanal em sílica gel Influence of organic solvents on adsorption of linalool and decanal on silica gel

    Directory of Open Access Journals (Sweden)

    Adriana Régia Cornélio

    2004-08-01

    Full Text Available Estudou-se a influência de solventes orgânicos (etanol, propanol e acetato de etila na isoterma de adsorção de uma solução-modelo do óleo essencial de laranja em sílica-gel. A solução-modelo constituiu-se de compostos oxigenados (linalol e decanal dissolvidos em d-limoneno (solvente. A influência da temperatura no processo de adsorção foi determinada para sistemas ternário (d-limoneno + linalol + decanal à temperatura de 298,15 K. Para o composto oxigenado decanal, os solventes que mais influenciaram no processo de adsorção foram o etanol e o acetato de etila; já para o linalol, todos os solventes estudados tiveram influência sobre o processo.The influence of organic solvents (ethanol, propanol and ethyl acetate on the isotherm of adsorption of model solutions of orange essential oil on silica gel was investigated. The model solution consisted of oxygenated compounds (linalool and decanal dissolved in d-limoneno. The influence of temperature on the process of adsorption was determined by ternary systems (d-limoneno + linalool + decanal at the temperature of 298,15 K . For the oxygenated compound decanal, the solvents that showed greater influence on the process of adsorption were ethanol and ethyl acetate, and for linalool all of the solvents studied were shown to influence the process.

  17. Mild hydration of didecyldimethylammonium chloride modified DNA by 1H-nuclear magnetic resonance and by sorption isotherm

    Science.gov (United States)

    Harańczyk, H.; Kobierski, J.; Nizioł, J.; Hebda, E.; Pielichowski, J.; Zalitacz, D.; Marzec, M.; El-Ghayoury, A.

    2013-01-01

    The gaseous phase hydration of deoxyribonucleic acid and didecyldimethylammonium chloride (C19H42ClN) complexes (DNA-DDCA) was observed using hydration kinetics, sorption isotherm, and high power nuclear magnetic resonance. Three bound water fractions were distinguished: (i) a very tightly bound water not removed by incubation over silica gel, (ii) a tightly bound water saturating with the hydration time t1h = (0.59 ± 0.04) h, and a loosely bound water fraction, (iii) with the hydration time t2h = (20.9 ± 1.3) h. Proton free induction decay was decomposed into the signal associated with the solid matrix of DNA-DDCA complex (T2S∗≈ 30 μs) and two liquid signal components coming from tightly bound (T2L1∗≈ 100 μs) and from loosely bound water fraction (T2L2∗≈ 1000 μs).

  18. Rare-earth doped YF{sub 3} nanocrystals embedded in sol-gel silica glass matrix for white light generation

    Energy Technology Data Exchange (ETDEWEB)

    Mendez-Ramos, J. [Departamento Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Santana-Alonso, A. [Departamento Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Yanes, A.C., E-mail: ayanesh@ull.e [Departamento Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Castillo, J. del [Departamento Fisica Basica, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain); Rodriguez, V.D. [Departamento Fisica Fundamental y Experimental, Electronica y Sistemas, Universidad de La Laguna, 38206 La Laguna, Tenerife (Spain)

    2010-12-15

    YF{sub 3} nanocrystals triply-doped with Yb{sup 3+}, Ho{sup 3+} and Tm{sup 3+} ions embedded in amorphous silica matrix have been successfully obtained by heat treatment of precursor sol-gel glasses for the first time to our knowledge and confirmed by X-ray diffraction and luminescence measurements. Simultaneous UV and visible efficient up-conversion emissions, with well-resolved Stark structure, under 980 nm infrared pump are observed, indicating the effective partition of rare-earth ions into a crystalline-like environment of the YF{sub 3} nanocrystals. Corresponding energy transfer mechanisms have been analyzed and overall colour emission has been quantified in terms of standard chromaticity diagram. By an adequate doping level and heat treatment temperature of precursor sol-gel glasses, a bright white colour has been accomplished, close to the standard equal energy white light illumination point, with potential applications in photo-electronic devices and information processing.

  19. Effects of crown ethers in nanocomposite silica-gel electrolytes on the performance of quasi-solid-state dye-sensitized solar cells

    KAUST Repository

    Huang, Kuan-Chieh

    2010-04-01

    The effects of crown ethers (CEs) on the performance of quasi-solid-state dye-sensitized solar cells (DSSCs) have been investigated. Nanocomposite silica was used to form gel matrices in the electrolytes, which contained lithium iodide (LiI) and iodine (I2) in 3-methoxypropionitrile (MPN) solvent. Three types of CEs, 12-crown-4 (12-C-4), 15-crown-5 (15-C-5), and 18-crown-6 (18-C-6) were used as additives to the gel electrolytes. DSSCs containing CEs showed enhancements in solar-to-electricity conversion efficiencies (η), with reference to the one without them. The crown ether, 15-C-5, with a size of cavity matching with the size of Li+ in the electrolyte rendered for its DSSC the best performance with an η of 3.60%, under 100 mW/cm2 illumination, as compared to 2.44% for the cell without any CE. Enhancements in the photovoltaic parameters of the cells with the CEs were explained based on the binding abilities of the CEs with lithium ions (Li+) in the electrolyte. Linear sweep voltammetry (LSV) measurements and electrochemical impedance spectra were used to substantiate the explanations. © 2009 Elsevier B.V. All rights reserved.

  20. One-pot preparation of silica-supported hybrid immobilized metal affinity adsorbent with macroporous surface based on surface imprinting coating technique combined with polysaccharide incorporated sol--gel process.

    Science.gov (United States)

    Li, Feng; Li, Xue-Mei; Zhang, Shu-Sheng

    2006-10-06

    A simple and reliable one-pot approach using surface imprinting coating technique combined with polysaccharide incorporated sol-gel process was established to synthesize a new organic-inorganic hybrid matrix possessing macroporous surface and functional ligand. Using mesoporous silica gel being a support, immobilized metal affinity adsorbent with a macroporous shell/mesoporous core structure was obtained after metal ion loading. In the prepared matrix, covalently bonded coating and morphology manipulation on silica gel was achieved by using one-pot sol-gel process starting from an inorganic precursor, -glycidoxypropyltrimethoxysiloxane (GPTMS), and a functional biopolymer, chitosan (CS) at the atmosphere of imprinting polyethylene glycol (PEG). Self-hydrolysis of GPTMS, self-condensation, and co-condensation of silanol groups (Si-OH) from siloxane and silica gel surface, and in situ covalent cross-linking of CS created an orderly coating on silica gel surface. PEG extraction using hot ammonium hydroxide solution gave a chemically and mechanically stabilized pore structure and deactivated residual epoxy groups. The prepared matrix was characterized by using X-ray energy dispersion spectroscopy (EDX), scanning electron microscopy (SEM) and mercury intrusion porosimetry. The matrix possessed a high capacity for copper ion loading. Protein adsorption performance of the new immobilized metal affinity adsorbent was evaluated by batch adsorption and column chromatographic experiment using bovine serum albumin (BSA) as a simple model protein. Under the optimized coating conditions, the obtained macroporous surface resulted in a fast kinetics and high capability for protein adsorption, while the matrix non-charged with metal ions offered a low non-specific adsorption.

  1. Improved Mobility Control for Carbon Dioxide (CO{sub 2}) Enhanced Oil Recovery Using Silica-Polymer-Initiator (SPI) Gels

    Energy Technology Data Exchange (ETDEWEB)

    Oglesby, Kenneth

    2014-01-31

    SPI gels are multi-component silicate based gels for improving (areal and vertical) conformance in oilfield enhanced recovery operations, including water-floods and carbon dioxide (CO{sub 2}) floods, as well as other applications. SPI mixtures are like-water when pumped, but form light up to very thick, paste-like gels in contact with CO{sub 2}. When formed they are 3 to 10 times stronger than any gelled polyacrylamide gel now available, however, they are not as strong as cement or epoxy, allowing them to be washed / jetted out of the wellbore without drilling. This DOE funded project allowed 8 SPI field treatments to be performed in 6 wells (5 injection wells and 1 production well) in 2 different fields with different operators, in 2 different basins (Gulf Coast and Permian) and in 2 different rock types (sandstone and dolomite). Field A was in a central Mississippi sandstone that injected CO{sub 2} as an immiscible process. Field B was in the west Texas San Andres dolomite formation with a mature water-alternating-gas miscible CO{sub 2} flood. Field A treatments are now over 1 year old while Field B treatments have only 4 months data available under variable WAG conditions. Both fields had other operational events and well work occurring before/ during / after the treatments making definitive evaluation difficult. Laboratory static beaker and dynamic sand pack tests were performed with Ottawa sand and both fields’ core material, brines and crude oils to improve SPI chemistry, optimize SPI formulations, ensure SPI mix compatibility with field rocks and fluids, optimize SPI treatment field treatment volumes and methods, and ensure that strong gels set in the reservoir. Field quality control procedures were designed and utilized. Pre-treatment well (surface) injectivities ranged from 0.39 to 7.9 MMCF/psi. The SPI treatment volumes ranged from 20.7 cubic meters (m{sup 3}, 5460 gallons/ 130 bbls) to 691 m{sup 3} (182,658 gallons/ 4349 bbls). Various size and types

  2. Simulating the Transition between Gel and Liquid-Crystal Phases of Lipid Bilayers : Dependence of the Transition Temperature on the Hydration Level

    NARCIS (Netherlands)

    Horta, Bruno A. C.; de Vries, Alex H.; Hunenberger, Philippe H.

    2010-01-01

    Explicit-solvent molecular dynamics (MD) simulations of the monoglyceride glycerol-1-monopalmitin (GMP, bilayer patch of 2 x 6 x 6 lipids) at different hydration levels (full, half, or quarter hydration) and at different temperatures (318 to 338 K) are reported. The 40 ns simulations (some extended

  3. Formation of magnesium silicate hydrate (M-S-H) cement pastes using sodium hexametaphosphate

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Tingting [Faculty of Infrastructure Engineering, Dalian University of Technology, Dalian 116024 (China); Department of Materials, Centre for Advanced Structural Ceramics, Imperial College London, South Kensington Campus, London SW7 2AZ (United Kingdom); Department of Civil and Environmental Engineering, Imperial College London, South Kensington Campus, London SW7 2AZ (United Kingdom); Vandeperre, Luc J. [Department of Materials, Centre for Advanced Structural Ceramics, Imperial College London, South Kensington Campus, London SW7 2AZ (United Kingdom); Cheeseman, Christopher R., E-mail: c.cheeseman@imperial.ac.uk [Department of Civil and Environmental Engineering, Imperial College London, South Kensington Campus, London SW7 2AZ (United Kingdom)

    2014-11-15

    Magnesium silicate hydrate (M-S-H) gel is formed by the reaction of brucite with amorphous silica during sulphate attack in concrete and M-S-H is therefore regarded as having limited cementing properties. The aim of this work was to form M-S-H pastes, characterise the hydration reactions and assess the resulting properties. It is shown that M-S-H pastes can be prepared by reacting magnesium oxide (MgO) and silica fume (SF) at low water to solid ratio using sodium hexametaphosphate (NaHMP) as a dispersant. Characterisation of the hydration reactions by x-ray diffraction and thermogravimetric analysis shows that brucite and M-S-H gel are formed and that for samples containing 60 wt.% SF and 40 wt.% MgO all of the brucites react with SF to form M-S-H gel. These M-S-H cement pastes were found to have compressive strengths in excess of 70 MPa.

  4. Hydration rate of obsidian.

    Science.gov (United States)

    Friedman, I; Long, W

    1976-01-30

    The hydration rates of 12 obsidian samples of different chemical compositions were measured at temperatures from 95 degrees to 245 degrees C. An expression relating hydration rate to temperature was derived for each sample. The SiO(2) content and refractive index are related to the hydration rate, as are the CaO, MgO, and original water contents. With this information it is possible to calculate the hydration rate of a sample from its silica content, refractive index, or chemical index and a knowledge of the effective temperature at which the hydration occurred. The effective hydration temperature can be either measured or approximated from weather records. Rates have been calculated by both methods, and the results show that weather records can give a good approximation to the true EHT, particularly in tropical and subtropical climates. If one determines the EHT by any of the methods suggested, and also measures or knows the rate of hydration of the particular obsidian used, it should be possible to carry out absolute dating to +/- 10 percent of the true age over periods as short as several years and as long as millions of years.

  5. Functionalisation of mesoporous silica gel with 2-[(phosphonomethyl)-amino]acetic acid functional groups. Characterisation and application

    Science.gov (United States)

    Caldarola, Dario; Mitev, Dimitar P.; Marlin, Lucile; Nesterenko, Ekaterina P.; Paull, Brett; Onida, Barbara; Bruzzoniti, Maria Concetta; Carlo, Rosa Maria De; Sarzanini, Corrado; Nesterenko, Pavel N.

    2014-01-01

    A new complexing adsorbent was prepared by chemical modification of mesoporous silica Kieselgel 60 (dp = 37-63 μm, average pore size 6 nm, specific surface area 425 m2 g-1) with 3-glycidoxypropyltrimethoxysilane and 2-[(phosphonomethyl)amino]acetic acid (PMA), commonly known as glyphosate. The prepared adsorbent was fully characterised using elemental analysis, thermal gravimetric analysis (TGA), acid-base potentiometric titration, Fourier Transform Infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption isotherms at 77 K (BET), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS). The concentration of bonded PMA groups calculated from the nitrogen content was 0.38 mmol per gram. The adsorption of transition metal ions on PMA functionalised silica (HEPMAS) was studied from aqueous solutions having different pH and the following selectivity was established, Zn(II) < Co(II) < Cd(II) < Mn(II) < Ni(II) < Cu(II). The calculated values of distribution coefficients D for the adsorption of ecotoxic metal ions on HEPMAS are 5.0 × 104, 4.9 × 105 and 2.6 × 104 for Zn(II), Pb(II) and Cd(II), respectively.

  6. Functionalisation of mesoporous silica gel with 2-[(phosphonomethyl)-amino]acetic acid functional groups. Characterisation and application

    Energy Technology Data Exchange (ETDEWEB)

    Caldarola, Dario [Department of Applied Science and Technology, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy); Australian Centre for Research on Separation Sciences (ACROSS), University of Tasmania, Hobart, Tasmania 7001 (Australia); Mitev, Dimitar P. [Australian Centre for Research on Separation Sciences (ACROSS), University of Tasmania, Hobart, Tasmania 7001 (Australia); Marlin, Lucile [Ecole Nationale Superieure des Ingenieurs en Arts Chimiques et Technologiquesm, Toulouse (France); Irish Separation Science Cluster, Dublin City University, Dublin (Ireland); Nesterenko, Ekaterina P. [Irish Separation Science Cluster, Dublin City University, Dublin (Ireland); Paull, Brett [Australian Centre for Research on Separation Sciences (ACROSS), University of Tasmania, Hobart, Tasmania 7001 (Australia); Onida, Barbara [Department of Applied Science and Technology, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy); CR-INSTM for Materials with Controlled Porosity (Italy); Bruzzoniti, Maria Concetta; Carlo, Rosa Maria De; Sarzanini, Corrado [Analytical Chemistry Department, University of Torino, Via P. Giuria 5, 10125 Torino (Italy); Nesterenko, Pavel N., E-mail: Pavel.Nesterenko@utas.edu.au [Australian Centre for Research on Separation Sciences (ACROSS), University of Tasmania, Hobart, Tasmania 7001 (Australia)

    2014-01-01

    A new complexing adsorbent was prepared by chemical modification of mesoporous silica Kieselgel 60 (d{sub p} = 37–63 μm, average pore size 6 nm, specific surface area 425 m{sup 2} g{sup −1}) with 3-glycidoxypropyltrimethoxysilane and 2-[(phosphonomethyl)amino]acetic acid (PMA), commonly known as glyphosate. The prepared adsorbent was fully characterised using elemental analysis, thermal gravimetric analysis (TGA), acid–base potentiometric titration, Fourier Transform Infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), nitrogen adsorption isotherms at 77 K (BET), scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM-EDS). The concentration of bonded PMA groups calculated from the nitrogen content was 0.38 mmol per gram. The adsorption of transition metal ions on PMA functionalised silica (HEPMAS) was studied from aqueous solutions having different pH and the following selectivity was established, Zn(II) < Co(II) < Cd(II) < Mn(II) < Ni(II) < Cu(II). The calculated values of distribution coefficients D for the adsorption of ecotoxic metal ions on HEPMAS are 5.0 × 10{sup 4}, 4.9 × 10{sup 5} and 2.6 × 10{sup 4} for Zn(II), Pb(II) and Cd(II), respectively.

  7. The experimental design approach to eluotropic strength of 20 solvents in thin-layer chromatography on silica gel.

    Science.gov (United States)

    Komsta, Łukasz; Stępkowska, Barbara; Skibiński, Robert

    2017-02-03

    The eluotropic strength on thin-layer silica plates was investigated for 20 chromatographic grade solvents available in current market. 35 model compounds were used as test subjects in the investigation. The use of modern mixture screening design allowed to estimate each solvent as a separate elution coefficient with an acceptable error of estimation (0.0913 of RM value). Additional bootstrapping technique was used to check the distribution and uncertainty of eluotropic estimates, proving very similar confidence intervals to linear regression. Principal component analysis proved that the only one parameter (mean eluotropic strength) is satisfactory to describe the solvent property, as it explains almost 90% of variance of retention. The obtained eluotropic data can be good appendix to earlier published results and their values can be interpreted in context of RM differences. Copyright © 2017 Elsevier B.V. All rights reserved.

  8. Molecular dynamics study on mechanism of preformed particle gel transporting through nanopores: Surface chemistry and heterogeneity

    Science.gov (United States)

    Cui, Peng; Zhang, Heng; Ma, Ying; Hao, Qingquan; Liu, Gang; Sun, Jichao; Yuan, Shiling

    2017-10-01

    The translocation behavior of preformed particle gel (PPG) in porous media is crucial for its application in enhanced oil recovery. By means of non-equilibrium molecular dynamics simulation, the translocation mechanism of PPG confined in different silica nanopores were investigated. The influence of surface chemistry and chemical heterogeneity of silica nanopore on the translocation process was revealed. As the degree of surface hydroxylation increases and the heterogeneity decreases, the pulling force needed to drive PPG decreases. We infer that the nanopore's surface (i.e. surface chemistry and heterogeneity) affects the translocation of PPG indirectly by forming different hydration layers.

  9. Effect of CdS nanoparticles on photoluminescence spectra of Tb3+ in sol–gel-derived silica glasses

    Indian Academy of Sciences (India)

    S Rai; L Bokatial

    2011-04-01

    CdS nanoparticles doped with Tb3+ were synthesized by sol–gel technique. The influence of CdS on the Tb3+ glass was studied by UV-Visible and luminescence spectroscopy. The luminescence intensity of the glasses increased significantly in the presence of CdS nanoparticles. Terbium ions excited into the ${}^{5}D_{3}$ level have a rich emission spectrum in the 400–700 nm range decaying to different ${}^{7}F_{J}$ levels. The intensity of violet and blue luminescence from ${}^{5}D_{3}$ level is highly dependent on Tb3+ concentration, on presence of CdS co-dopant and annealing conditions.

  10. Vapor-Liquid Sol-Gel Approach to Fabricating Highly Durable and Robust Superhydrophobic Polydimethylsiloxane@Silica Surface on Polyester Textile for Oil-Water Separation.

    Science.gov (United States)

    Su, Xiaojing; Li, Hongqiang; Lai, Xuejun; Zhang, Lin; Wang, Jing; Liao, Xiaofeng; Zeng, Xingrong

    2017-08-23

    Large-scale fabrication of superhydrophobic surfaces with excellent durability by simple techniques has been of considerable interest for its urgent practical application in oil-water separation in recent years. Herein, we proposed a facile vapor-liquid sol-gel approach to fabricating highly durable and robust superhydrophobic polydimethylsiloxane@silica surfaces on the cross-structure polyester textiles. Scanning electron microscopy and Fourier transform infrared spectroscopy demonstrated that the silica generated from the hydrolysis-condensation of tetraethyl orthosilicate (TEOS) gradually aggregated at microscale driven by the extreme nonpolar dihydroxyl-terminated polydimethylsiloxane (PDMS(OH)). This led to construction of hierarchical roughness and micronano structures of the superhydrophobic textile surface. The as-fabricated superhydrophobic textile possessed outstanding durability in deionized water, various solvents, strong acid/base solutions, and boiling/ice water. Remarkably, the polyester textile still retained great water repellency and even after ultrasonic treatment for 18 h, 96 laundering cycles, and 600 abrasion cycles, exhibiting excellent mechanical robustness. Importantly, the superhydrophobic polyester textile was further applied for oil-water separation as absorption materials and/or filter pipes, presenting high separation efficiency and great reusability. Our method to construct superhydrophobic textiles is simple but highly efficient; no special equipment, chemicals, or atmosphere is required. Additionally, no fluorinated slianes and organic solvents are involved, which is very beneficial for environment safety and protection. Our findings conceivably stand out as a new tool to fabricate organic-inorganic superhydrophobic surfaces with strong durability and robustness for practical applications in oil spill accidents and industrial sewage emission.

  11. Synthesis of magnetic FexOy@silica-pillared clay (SPC) composites via a novel sol-gel route for controlled drug release and targeting.

    Science.gov (United States)

    Mao, Huihui; Liu, Xiaoting; Yang, Jihe; Li, Baoshan; Yao, Chao; Kong, Yong

    2014-07-01

    Novel magnetic silica-pillared clay (SPC) materials with an ordered interlayered mesopore structure were synthesized via a two-step method including gallery molecular self-assembly and sol-gel magnetic functionalization, resulting in the formation of FexOy@SPC composites. Small-angle XRD, TEM and N2 adsorption-desorption isotherms results show that these composites conserved a regular layered and ordered mesoporous structure after the formation of FexOy nanoparticles. Wide-angle XRD and XPS analyses confirmed that the FexOy generated in these mesoporous silica-pillared clay hosts is mainly composed of γ-Fe2O3. Magnetic measurements reveal that these composites with different γ-Fe2O3 loading amounts possess super-paramagnetic properties at 300K, and the saturation magnetization increases with increasing Fe ratio loaded. Compared to the pure SPC, the in vitro drug release rate of the FexOy@SPC composites was enhanced due to the fact that the intensities of the SiOH bands on the pore surface of SPC decrease after the generation of FexOy. However, under an external magnetic field of 0.15T, the drug release rate of the FexOy@SPC composites decreases dramatically owing to the aggregation of the magnetic FexOy@SPC particles triggered by non-contact magnetic force. The obtained FexOy@SPC composites imply the possibility of application in magnetic drug targeting. Copyright © 2014 Elsevier B.V. All rights reserved.

  12. Matrix effects on the photocatalytic oxidation of alcohols by [nBu4N]4W10O32 incorporated into sol-gel silica.

    Science.gov (United States)

    Molinari, Alessandra; Bratovcic, Amra; Magnacca, Giuliana; Maldotti, Andrea

    2010-09-07

    Two heterogeneous photocatalysts have been prepared by entrapment of [nBu(4)N](4)W(10)O(32) in a silica matrix, through a sol-gel procedure: SiO(2)/W30% and SiO(2)/W10% with 30% and 10% of decatungstate, respectively. They are characterized by the presence of micropores of about 7 A and 15 A and mesopores of about 25 A. Due to different preparation procedures, SiO(2)/W10% presents a more remarkable porous network than SiO(2)/W30%. The morphological features of SiO(2)/W30% and SiO(2)/W10% differ from those of their parent material SiO(2)/W0%, indicating that incorporation of the decatungstate induces a significant modification of the porous texture of the siliceous material. These photocatalysts demonstrate good stability in the oxygen-assisted photooxidation of 1-pentanol and 3-pentanol, which have been chosen as models of primary and secondary aliphatic alcohols. In particular, photoexcitation (lambda > 290 nm, 25 degrees C, 760 torr of O(2)) leads to conversion of these two substrates to pentanal or 3-pentanone, with a mass balance of about 90%. There is a strong effect of the solid support on the reactivity of the two alcoholic substrates. In particular, oxidation of 1-pentanol with SiO(2)/W10% is about four times faster than with [nBu(4)N](4)W(10)O(32) in homogeneous solution. Preferential adsorption phenomena, due to the hydrophilic character of silica explain the photocatalytic properties of the two heterogeneous systems, because adsorption favours the contact between the photoexcited decatungstate and the primary OH group of 1-pentanol. Moreover, some kind of shape selectivity, due to the microporous structure of the investigated materials, likely contributes to control the conversion yields.

  13. Sensitive detection of influenza viruses with Europium nanoparticles on an epoxy silica sol-gel functionalized polycarbonate-polydimethylsiloxane hybrid microchip.

    Science.gov (United States)

    Liu, Jikun; Zhao, Jiangqin; Petrochenko, Peter; Zheng, Jiwen; Hewlett, Indira

    2016-12-15

    In an effort to develop new tools for diagnosing influenza in resource-limited settings, we fabricated a polycarbonate (PC)-polydimethylsiloxane (PDMS) hybrid microchip using a simple epoxy silica sol-gel coating/bonding method and employed it in sensitive detection of influenza virus with Europium nanoparticles (EuNPs). The incorporation of sol-gel material in device fabrication provided functionalized channel surfaces ready for covalent immobilization of primary antibodies and a strong bonding between PDMS substrates and PC supports without increasing background fluorescence. In microchip EuNP immunoassay (µENIA) of inactivated influenza viruses, replacing native PDMS microchips with hybrid microchips allowed the achievement of a 6-fold increase in signal-to-background ratio, a 12-fold and a 6-fold decreases in limit-of-detection (LOD) in influenza A and B tests respectively. Using influenza A samples with known titers, the LOD of influenza µENIA on hybrid microchips was determined to be ~10(4) TCID50 titer/mL and 10(3)-10(4) EID50 titer/mL. A comparison test indicated that the sensitivity of influenza µENIA enhanced using the hybrid microchips even surpassed that of a commercial laboratory influenza ELISA test. In addition to the sensitivity improvement, assay variation was clearly reduced when hybrid microchips instead of native PDMS microchips were used in the µENIA tests. Finally, infectious reference viruses and nasopharyngeal swab patient specimens were successfully tested using μENIA on hybrid microchip platforms, demonstrating the potential of this unique microchip nanoparticle assay in clinical diagnosis of influenza. Meanwhile, the tests showed the necessity of using nucleic acid confirmatory tests to clarify ambiguous test results obtained from prototype or developed point-of-care testing devices for influenza diagnosis.

  14. Structural and optical characterization of oxygenated CdTe/Sm{sup 3+} in sol-gel silica glasses

    Energy Technology Data Exchange (ETDEWEB)

    Mathew, Siby; Rejikumar, P.R.; Adiyodi, Amrutha K.; Jyothy, P.V. [School of Pure and Applied Physics, Mahatma Gandhi University, Kottayam 686560 (India); Unnikrishnan, N.V. [School of Pure and Applied Physics, Mahatma Gandhi University, Kottayam 686560 (India)], E-mail: nvu50@yahoo.co.in

    2008-12-20

    Oxygenated cadmium telluride co-doped with rare earth element samarium is prepared by sol-gel method. Sample is air annealed at 200, 500 and 800 deg. C. The absorption and fluorescence spectra are analysed using Judd-Ofelt analysis to obtain J-O parameters. X-ray spectroscopy analysis shows the presence of thermally grown CdTeO{sub 3} phase developed at the expense of CdTe phase on heat treatment for samples annealed at 800 deg. C. The FT-IR spectrum of the sample is taken at different annealing temperatures and the assignments of the absorption bands are compiled which shows the gradual evolution of the rigid glassy network formed. Enhanced fluorescence from air annealed Co-doped samples are also investigated.

  15. Optimization of synthesis parameters of mesoporous silica sol-gel thin films for application on 2024 aluminum alloy substrates

    Science.gov (United States)

    Recloux, Isaline; Debliquy, Marc; Baroni, Alexandra; Paint, Yoann; Lanzutti, Alex; Fedrizzi, Lorenzo; Olivier, Marie-Georges

    2013-07-01

    Silica mesoporous films were synthesized via Evaporation Induced Self-Assembly (EISA) using Pluronic P123 as templating agent and were applied on 2024 aluminum alloy for surface treatment applications. The removal of the P123 from the film required to convert the mesostructured film into a mesoporous film was particularly studied and optimized in order to be compatible with the use of an aluminum substrate. In this work, two different kinds of removal treatments were compared: calcination at high temperatures and UV/ozone treatment. Indeed, a minimum temperature of 275 °C has to be reached to completely remove the templating agent from the film. However, this treatment also leads to a decrease in mechanical properties of the aluminum substrate. In opposition, the removal by UV/ozone illumination allows getting mesoporous films at room temperature with important pore volume and high specific surface area without impacting mechanical properties of the aluminum. The effect of these treatments on mechanical properties of bare aluminum was followed by microhardness. The development of the porosity inside the film due to the elimination of the P123 was measured by combining analytical techniques (Fourier transform infrared spectroscopy FTIR, radio-frequency glow discharge optical emission spectroscopy RF-GDOES), electrochemical impedance spectroscopy (EIS) and adsorption porosimetry using a quartz crystal microbalance.

  16. Investigation of bioactivity, biocompatibility and thermal behavior of sol–gel silica glass containing a high PEG percentage

    Energy Technology Data Exchange (ETDEWEB)

    Catauro, M., E-mail: michelina.catauro@unina2.it [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29, 81031 Aversa (Italy); Renella, R.A.; Papale, F. [Department of Industrial and Information Engineering, Second University of Naples, Via Roma 29, 81031 Aversa (Italy); Vecchio Ciprioti, S. [Department of Basic and Applied Science for Engineering, Sapienza University of Rome, Via del Castro Laurenziano 7, Building RM017, I-00161 Rome (Italy)

    2016-04-01

    SiO{sub 2}/PEG organic–inorganic hybrid materials, which contain 60 or 70 weight percentage of PEG, were synthesized by the sol–gel technique. The materials were characterized and subjected to various tests to assess their application in the biomedical field. The evaluation of their morphology by scanning electron microscopy (SEM) confirms the homogeneity of the samples on the nanometer scale. Fourier transform infrared spectroscopy (FT-IR) indicated that the two components of the hybrids (SiO{sub 2} and PEG) are linked by hydrogen bonds. This feature makes them class I hybrids. Simultaneous thermogravimetry/differential thermal analysis (TG/DTA) was used to investigate their thermal behavior and to establish the best temperatures for their pre-treatment. The fundamental properties that a material must have to be used in the biomedical field are biocompatibility and bioactivity. The formation of a hydroxyapatite layer was observed on the hybrid surface by SEM/EDX and FTIR after soaking in simulated body fluid. This indicates that the materials are able to bond to bone tissue. Moreover, the biocompatibility of SiO{sub 2}/PEG hybrids was assessed by performing WST-8 cytotoxicity tests on fibroblast cell NIH 3T3 after 24 h of exposure. The cytotoxicity tests highlight that the cell viability is affected by the polymer percentage. The results showed that the synthesized materials were bioactive and biocompatible. Therefore, the results obtained are encouraging for the use of the obtained hybrids in dental or orthopedic applications. - Highlights: • SiO{sub 2}/PEG hybrid biomaterials synthesized by sol–gel method at high PEG percentage • Chemical, thermal and morphological characterization of hybrid materials • Biological characterizations with WST-8 cytotoxicity tests • Bioactivity characterizations of hybrid materials with high PEG percentage.

  17. Synthesis and Characterization of Bimodal Mesoporous Silica

    Institute of Scientific and Technical Information of China (English)

    ZHANG Xiaofang; GUO Cuili; WANG Xiaoli; WU Yuanyuan

    2012-01-01

    Mesoporous silica with controllable bimodal pore size distribution was synthesized with cetyltrimethylammonium bromide (CTAB) as chemical template for small mesopores and silica gel as physical template for large mesopores.The structure of synthesized samples were characterized by Fourier transform infrared (FT-IR) spectroscopy,X-ray diffraction (XRD),scanning electron microscopy (SEM),transmission electron microscopy (TEM) and N2 adsorption-desorption measurements.The experimental results show that bimodal mesoporous silica consists of small mesopores of about 3 nm and large mesopores of about 45 nm.The small mesopores which were formed on the external surface and pore walls of the silica gel had similar characters with those of MCM-41,while large mesopores were inherited from parent silica gel material.The pore size distribution of the synthesized silica can be adjusted by changing the relative content of TEOS and silica gel or the feeding sequence of silica gel and NH4OH.

  18. 溶液吸附法测定硅胶表面分形值%Surface Fractal Measurement for Silica Gel by Adsorption Method

    Institute of Scientific and Technical Information of China (English)

    邱诚; 李玫

    2014-01-01

    The degree of the surface fractal of silica gel is measured by adsorption of methylene blue(MB), crystal violet, Safranin-T, acid red-94 and cresol red.The result of the degree is about 2.002.Adsorption capacity of equilibrium is substituted for that of limit, so the calculating process is simple and clear.%根据一种中孔硅胶对亚甲基蓝、结晶紫、番红花红T、酸性红94和甲酚红等五种染料的吸附数据结果计算了该硅胶表面分形值D。由吸附数据得出的该硅胶表面的分形值D等于2.002。利用平衡吸附量nm取代极限吸附量nl,求得硅胶表面分形值D,计算过程更加简明。

  19. Molecularly imprinted polymers on the surface of silica microspheres via sol-gel method for the selective extraction of streptomycin in aqueous samples.

    Science.gov (United States)

    Junjie, Li; Mei, Yang; Danqun, Huo; Changjun, Hou; Xianliang, Li; Guomin, Wang; Dan, Feng

    2013-03-01

    Streptomycin-imprinted silica microspheres were prepared by combining a surface molecular-imprinting technique with the sol-gel method. A mixture of tetrahydrofuran, ethanol, and water (6:1:1, v/v/v) was selected as dispersing solvent while 3-aminopropyltriethoxysilane and triethoxyphenylsilane acted as functional monomers, and tetraethyl orthosilicate as a cross-linker. Characterization of the molecularly imprinted polymers was conducted using scanning electron microscope and dynamic binding experiments. As compared to the nonimprinted polymers, the imprinted polymers exhibited a higher degree of saturated adsorption volume up to 26.3 mg/g, and better selectivity even in an aqueous solution with interfering compounds, including dihydrostreptomycin, neomycin, and tetracycline. The adsorption ability and selectivity were observed to be influenced by the mole ratio of 3-aminopropyltriethoxysilane and triethoxyphenylsilane. Feasibility of the polymers to be used for actual application was also evaluated with spiked samples, indicating great potential for large-scale applications. Moreover, the streptomycin-imprinted polymers can be repeatedly used for 12 cycles without losing original performance, which is beneficial for commercial use.

  20. Electrochemical properties of the hexacyanoferrate(II)–ruthenium(III) complex immobilized on silica gel surface chemically modified with zirconium(IV) oxide

    Energy Technology Data Exchange (ETDEWEB)

    Panice, Lucimara B.; Oliveira, Elisangela A. de; Filho, Ricardo A.D. Molin; Oliveira, Daniela P. de [Departamento de Química, Universidade Estadual de Maringá, Av. Colombo, 5790, 87020-900 Maringá, PR (Brazil); Lazarin, Angélica M., E-mail: amlazarin2@uem.br [Departamento de Química, Universidade Estadual de Maringá, Av. Colombo, 5790, 87020-900 Maringá, PR (Brazil); Andreotti, Elza I.S.; Sernaglia, Rosana L. [Departamento de Química, Universidade Estadual de Maringá, Av. Colombo, 5790, 87020-900 Maringá, PR (Brazil); Gushikem, Yoshitaka [Instituto de Química, Universidade Estadual de Campinas, Caixa Postal 6154, 13084-971 Campinas, São Paulo (Brazil)

    2014-10-15

    Highlights: • The cyano-bridged mixed valence ruthenium composite material was synthesized. • This newly synthesized compound was incorporated into a carbon paste electrode. • The electrode did not show significant changes in response after six months of use. • The modified electrode is very stable and reproducible. • The electrode sensor was successfully applied for ascorbic acid determination. - Abstract: The chemically modified silica gel with zirconium(IV) oxide was used to immobilize the [Fe(CN){sub 6}]{sup 4−} complex ion initially. The reaction of this material with [Ru(edta)H{sub 2}O]{sup −} complex ion formed the immobilized cyano-bridged mixed valence ruthenium complex, (≡Zr){sub 5}[(edta)RuNCFe(CN){sub 5}]. This material was incorporated into a carbon paste electrode and, its electrochemical properties were investigated. However, for an ascorbic acid solution, an enhancement of the anodic peak current was detected due to electrocatalytic oxidation. The electrode presented the same response for at least 150 successive measurements, with a good repeatability. The modified electrode is very stable and reproducible. The sensor was applied for ascorbic acid determination in pharmaceutical preparation with success.

  1. Mesoporous Silica Gel-Based Mixed Matrix Membranes for Improving Mass Transfer in Forward Osmosis: Effect of Pore Size of Filler.

    Science.gov (United States)

    Lee, Jian-Yuan; Wang, Yining; Tang, Chuyang Y; Huo, Fengwei

    2015-11-23

    The efficiency of forward osmosis (FO) process is generally limited by the internal concentration polarization (ICP) of solutes inside its porous substrate. In this study, mesoporous silica gel (SG) with nominal pore size ranging from 4-30 nm was used as fillers to prepare SG-based mixed matrix substrates. The resulting mixed matrix membranes had significantly reduced structural parameter and enhanced membrane water permeability as a result of the improved surface porosity of the substrates. An optimal filler pore size of ~9 nm was observed. This is in direct contrast to the case of thin film nanocomposite membranes, where microporous nanoparticle fillers are loaded to the membrane rejection layer and are designed in such a way that these fillers are able to retain solutes while allowing water to permeate through them. In the current study, the mesoporous fillers are designed as channels to both water and solute molecules. FO performance was enhanced at increasing filler pore size up to 9 nm due to the lower hydraulic resistance of the fillers. Nevertheless, further increasing filler pore size to 30 nm was accompanied with reduced FO efficiency, which can be attributed to the intrusion of polymer dope into the filler pores.

  2. The Preparation of Porous Sol-Gel Silica with Metal Organic Framework MIL-101(Cr) by Microwave-Assisted Hydrothermal Method for Adsorption Chillers

    Science.gov (United States)

    Uma, Kasimayan; Pan, Guan-Ting; Yang, Thomas C.-K.

    2017-01-01

    Metal organic framework (MOF) of MIL-101(Cr)-Silica (SiO2) composites with highly mesoporous and uniform dispersions were synthesized by a microwave-assisted hydrothermal method followed by the sol-gel technique. Water vapor adsorption experiments were conducted on the MIL-101(Cr)-SiO2 composites for industrial adsorption chiller applications. The effects of MIL-101(Cr)-SiO2 mixing ratios (ranging from 0% to 52%), the surface area and amount of Lewis and Brønsted sites were comprehensively determined through water vapor adsorption experiments and the adsorption mechanism is also explained. The BET and Langmuir results indicate that the adsorption isotherms associated with the various MIL-101(Cr)-SiO2 ratios demonstrated Type I and IV adsorption behavior, due to the mesoporous structure of the MIL-101(Cr)-SiO2. It was observed that the increase in the amount of Lewis and Brønsted sites on the MIL-101(Cr)-SiO2 composites significantly improves the water vapor adsorption efficiency, for greater stability during the water vapor adsorption experiments. PMID:28772969

  3. Mesoporous Silica Gel-Based Mixed Matrix Membranes for Improving Mass Transfer in Forward Osmosis: Effect of Pore Size of Filler

    Science.gov (United States)

    Lee, Jian