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PubMed2005

Preparation and characterisation of anion-exchange latex-coated silica monoliths for capillary electrochromatography.

Silica monoliths coated with functionalised latex particles have been prepared for use in monolithic ion-exchange capillary electrochromatography (IE-CEC) for the separation of inorganic anions. The ion-exchange monoliths were prepared using 70 nm quaternary ammonium, anion-exchange latex particles, which were bound electrostatically to a monolithic silica skeleton synthesised in a fused silica capillary. The resulting stationary phases were characterised in terms of their chromatographic performance and capacity. The capacity of a 50 microm diameter 25 cm latex-coated silica monolith was found to be 0.342 nanoequivalents and 80,000 theoretical plates per column were typically achieved for weakly retained anions, with lower efficiency being observed for analytes exhibiting strong ion-exchange interaction with the stationary phase. The electroosmotic flow (EOF) was reversed after the latex-coating was applied (-25.96 m2 V(-1) s(-1), relative standard deviation (RSD) 2.8%) and resulted in anions being separated in the co-EOF mode. Ion-exchange interactions between the analytes and the stationary phase were manipulated by varying the ion-exchange selectivity coefficient and the concentration of a competing ion (phosphate or perchlorate) present in the electrolyte. Large concentrations of competing ion (greater than 1M phosphate or 200 mM perchlorate) were required to completely suppress ion-exchange interactions, which highlighted the significant retention effects that could be achieved using monolithic columns compared to open tubular columns, without the problems associated with particle-packed columns. The latex-coated silica monoliths were easily produced in bulk quantities and performed reproducibly in acidic electrolytes. The high permeability and beneficial phase ratio makes these columns ideal for micro-LC and preconcentration applications.

Chromatography, Ion Exchange↗
PubMed2006

Development of acid stable, hyper-crosslinked, silica-based reversed-phase liquid chromatography supports for the separation of organic bases.

A new generation of extremely acid stable "hyper-crosslinked" (HC) phases have been developed with good plate counts for basic drug separations. In our previous work, we successfully developed an approach for synthesizing HC stationary phases on silica substrates using aluminum trichloride catalyzed Friedel-Crafts (F-C) chemistry to improve the stability of silica-based RPLC stationary phases at low pH. However, the performance of basic analytes on these HC phases under acidic conditions was unusually poor compared to that of conventional silica-based C18 phases. The effects of the specific F-C catalysts used and the specific silica substrate on the chromatographic properties of HC phases have been studied. Modified synthetic strategies that give both good observed plate counts for basic analytes under acidic conditions and very good low pH stability without compromising other chromatographic properties of the hyper-crosslinked phases have been developed. Replacement of aluminum trichloride with tin tetrachloride as the catalyst for the F-C chemistry and use of a very high purity silica result in significantly improved plate counts for basic analytes. In formic acid buffered mobile phases, which are highly compatible with electrospray ionization LC-MS, basic analytes showed much better performance on the tin tetrachloride catalyzed HC phases than on any conventional commercial phase tested. The tin tetrachloride catalyzed HC phase is as stable as the original aluminum trichloride catalyzed HC phases, and much more stable than the bench mark acid stable commercial phase.

Acids↗
PubMed2006

Protein concentration and adsorption time effects on fibrinogen adsorption at heparinized silica interfaces.

Heparin was modified with adipic dihydrazide and covalently linked to surface-activated silica wafers. X-ray photoelectron spectroscopy was used at each stage of derivatization and showed that successful immobilization had taken place. Surfaces were imaged with atomic force microscopy to determine the uniformity of the heparin layer as well as its thickness. In situ ellipsometry was used to estimate layer thickness as well, and to study protein concentration and adsorption time effects on the adsorption and elution kinetics exhibited by human plasma fibrinogen. The adsorbed amount of fibrinogen increased with time and concentration on each type of surface. Under all experimental conditions, fibrinogen adsorbed at a lower rate and to a lower extent on heparinized as compared to unheparinized silica. In addition, buffer elution experiments showed that fibrinogen was less tightly bound to heparinized silica. In order to examine behavior relative to fibrinogen mobility at these interfaces, the sequential adsorption of fibrinogen was recorded. The difference in adsorption rates between the first and second adsorption cycles, evaluated at identical mass density, indicated that post-adsorptive molecular rearrangements had taken place. In general, higher solution concentration and longer adsorption time in the first adsorption step led to more rearrangement, and these history dependent effects were more pronounced on the heparinized silica. These rearrangements are suggested to involve clustering of adsorbed fibrinogen, in this way increasing the amount of unoccupied area at the interface. These rearrangements were presumably facilitated on the heparinized silica by enhanced lateral mobility of fibrinogen at this negatively charged, highly hydrophilic interface.

Adipates↗
PubMed2006

The effect of five silane coupling agents on the bond strength of a luting cement to a silica-coated titanium.

OBJECTIVES: The adhesive performance of five silane coupling agents in adhering resin composite cement (3M ESPE) to silica-coated titanium was evaluated. Titanium was tribochemically silica-coated by using the Rocatec system. METHODS: Two volume percent solutions of 3-acryloyloxypropyltrimethoxysilane (Toray Dow Corning Silicone), N-[3-(trimethoxysilyl)propylethylenediamine] (Dow Corning), 3-mercaptopropyltrimethoxysilane (Toray Dow Corning Silicone) and bis-[3-(triethoxysilyl)propyl]polysulfide (Dow Corning) were prepared in 95 vol.% acidified ethanol and allowed to activate (hydrolyze). A pre-activated ca. 2 vol.% 3-methacryloyloxypropyltrimethoxysilane (ESPE Sil) was used as a control. The silanes were applied onto silica-coated titanium slides. Chemical activation reactions of the silanes were monitored by Fourier transform infrared spectrometry (Perkin-Elmer Spectrum One). RelyX ARC (3M ESPE) resin composite cement stubs were applied and photo-polymerized onto silica-coated titanium. The specimens were thermo-cycled (6000 cycles, 5-55 degrees C). RESULTS: Statistical analysis (ANOVA) showed that the highest shear bond strength (n=8 per group) value after thermocycling, 14.8 MPa (S.D. 3.8 MPa), was obtained with 2.0 vol.% 3-acryloyloxypropyltrimethoxysilane. Silanization and results with 3-methacryloyloxypropyltrimethoxysilane (control, ESPE Sil) did not statistically differ from 3-acryloyloxypropyltrimethoxysilane, 14.2 MPa (S.D. 5.8). The lowest shear bond strength was 7.5 (S.D. 1.9) MPa for N-[3-(trimethoxysilyl)propylethylenediamine] and 7.5 (S.D. 2.5) MPa for bis-[3-(triethoxysilyl)propyl]polysulfide. Both the type of silane (p<0.001) and storage conditions affected significantly the shear bond strength values (p<0.001). All silanes became activated according to the infrared spectroscopic analysis. SIGNIFICANCE: Silanization with 3-acryloyloxypropyltrimethoxysilane or 3-mercaptopropyltrimethoxysilane might offer an alternative for bonding a luting cement to silica-coated titanium.

Acrylates↗
PubMed2004

In vitro effects on macrophages induced by noncytotoxic doses of silica particles possibly relevant to ambient exposure.

The RAW 246.7 macrophage cell line was exposed in vitro to aged crystalline silica particles of respirable size for 24 h at a range of doses starting from 15 microg/2 x 10(6) cells, which is a realistic exposure level of macrophages in the airways of ambiently exposed individuals. The particle sample used for the experiments was prepared to mimic some aspects of ambient crystalline silica particles: size distribution, morphology, and surface reactivity. Our purpose was to determine whether a nontoxic quartz load comparable to that of ambient exposure would be able to induce macrophage activation and impairment of the phagocytic ability, factors altering the lung's capacity to deal with increased particle loads (as occurs during high-pollution episodes) or infections and affecting the local and systemic responses through the release of biologically active compounds (cytokines, reactive oxygen species, NO, isoprostanes). Exposure of RAW 264.7 cells to aged silica particles induced macrophage activation (evidenced by the morphological features observed with scanning electron microscopy and by the release of TNF-alpha and IL-6) and impairment of phagocytosis of test particles, even at noncytotoxic doses. The reduction of the phagocytic function of the cells after silica treatment was dose-dependent, as evidenced by an increase of the population of unphagocytic cells, paralleled by a decrease of the actively phagocytizing cell population. We evaluated the oxidative stress induced by aged silica particles, quantifying the peroxidation products (8-isoprostanes) in the culture media of treated cells, and found a strong release at low doses. Isoprostanes are a complex family of compounds which have been used as in vivo markers of lipid peroxidation in human disorders, but that, as far as we know, have never been evaluated in relation to airborne particulate matter exposure. Lipid peroxides are involved in various cellular events in the inflammatory response, and isoprostanes are also supposed to exert important biological actions on airway and pulmonary vascular smooth muscles and on platelets.

Air Pollutants↗
PubMed2004

Preparation of multilayered gold-silica-polystyrene core-shell particles by seeded polymerization.

A preparation method for multilayered gold-silica-polystyrene core-shell composite particles is proposed. The gold-silica core-shell particles of 192-nm-sized, synthesized by coating the 18-nm-sized gold particles with silica by a seeded growth technique, were used as cores for succeeding polystyrene coating. After surface modification of gold-silica composite particles by methacryloxypropyltrimethoxysilane (MPTMS), polymerizations of styrene (0.16-0.4 M) were conducted with 8 x 10(-3) M of potassium persulfate initiator in the presence of 1 x 10(-3) M of sodium p-styrenesulfonate anionic monomer. Multilayered core-shell gold-silica-polystyrene particles that contained a single core could be obtained. The coefficient of variation of size distribution (CV) of the composite particles was less than 7%, and polystyrene shell thickness was in a range of 193 to 281 nm.

Gold↗
PubMed2005

Effect of surfactant on particle morphology for liquid phase deposition of submicron silica.

Liquid phase deposition (LPD) of silica from soluble silicates has been performed in the presence of dodecyltrimethylammonium bromide (DTAB), sodium dodecyl sulfate (SDS) and sodium dodecylbenzyl sulfate (SDBS). The morphology of the silica varies between semi-ordered uniform spheres to low porosity agglomerates, with the choice and concentration of the surfactants. The agglomerate structures depend on the charge of the surfactant (and hence the retention of micelles under acidic LPD conditions and/or the ionic character of the surfactant solution), the critical micelle concentration (as compared to the concentration of the silica precursor), and the ionic strength of the solution. The application of surfactant micelles as templates for LPD silica is counter to a previous proposal that suggested the ionic strength of the silicate solution would cause the collapse of the ionic vesicles. The size of spherical silica particles is controlled by the relative concentration of the surfactant and the LPD precursor.

Journal Article↗
PubMed2005

The interaction at the solid/liquid interface of 2,4-dichlorophenoxyacetic acid with silica modified by reaction with ammonia gas.

A method for the attachment of ammonia to modified silica gel has been developed. In the first step, tetraethylorthosilicate and (3-glycidoxypropyl)trimethoxysilane were co-condensed in the presence of n-dodecylamine, a neutral surfactant template, to produce a modified mesoporous silica. The epoxy group incorporated into the mesoporous silica was opened by ammonia gas thus introducing amine chelate groups covalently bound to the inorganic surface. The modified material contained 1.13+/-0.06 mmol of amine per gram of silica, exhibited a surface area of 831+/-29 m(2)g(-1) and a porous diameter of 1.95 nm. Infrared, 29Si and 13C NMR spectra were in agreement with the proposed structure of the modified mesoporous silica in the solid state. This ordered organic-inorganic hybrid presented a high capacity for the removal of the agrochemical 2,4-dichlorophenoxyacetic acid from water: the DeltaH and DeltaG values for the interaction were determined to be -110.61 and -9.37 kJ mol(-1), respectively.

Journal Article↗
PubMed2005

A simple FTIR technique for estimating the surface area of silica powders and films.

A simple technique using FTIR spectroscopy to estimate the surface area of porous and non-porous silica powders is presented. The surface area is estimated by comparing the integrated area of the band due to isolated silanol groups on different silicas. We have found that by using a fumed silica as a calibrant, an accuracy of about 7% in the surface area of several silica materials is obtained when compared to the surface area computed by BET nitrogen adsorption techniques. The FTIR technique for computing surface area is simple and takes very little time to complete the analysis. The principle advantage of this method is that it enables surface area measurements of silica films on porous supports. To the best of our knowledge, there are no other methods that provide this information.

Journal Article↗
PubMed2005

Surface modification of silica nanoparticles by UV-induced graft polymerization of methyl methacrylate.

In this study we modified the surface of silica nanoparticles with methyl methacrylate by UV-induced graft polymerization. It is a surface-initiated polymerization reaction induced by ultraviolet irradiation. The resulting organic-inorganic nanocomposites were near-monodisperse and fabricated without homopolymerization of the monomer. Substantial increase in mean particle size was observed by SEM image analysis after UV-induced grafting of methyl methacrylate onto pure silica particles. FT-Raman spectroscopy and X-ray photoelectron spectroscopy studies of these materials revealed the successful grafting of methyl methacrylate onto the silica surface. The formation of a covalent bond between the grafted PMMA chains and silica surface was indicated by FT-Raman spectra. Thermogravimetric analysis of the PMMA-grafted silica particles indicated the polymer contents in good agreement with SEM photographs.

Nanoparticles↗
PubMed2005

Synthesis of high surface area Al-containing mesoporous silica from calcined and acid leached kaolinites as the precursors.

Al-containing mesoporous silicas were synthesized by hydrothermal treatment of microporous silica prepared by selectively acid leached metakaolinites with Si/Al = 3.9-92.5 mixed with a surfactant of cetyltrimethylammonium bromide (CTABr). The specific surface area of the products increased with higher surfactant/microporous silica (surf/Si) ratio and Si/Al ratio of the microporous silica, reaching about 1400 m2/g at CTABr/Si 0.1 and Si/Al 40. The XRD patterns of these products show a hexagonal (100) peak with the lattice parameter a0=4.2-4.3 nm and the N2 adsorption isotherms show steep increase of adsorption between relative pressure of 0.3 and 0.4. Hexagonal mesoporous microstructure is observed by high resolution TEM. The pore size distributions of the products show a sharp peak at 2.8 nm by the BJH method. The high specific surface area of the present mesoporous samples is attributed to the lower matrix density and surface roughness of mesopore wall. The highest specific surface area of the products reached up to 1420 m2/g and this value is apparently higher than those reported in hexagonal mesoporous silicas. A unique microporous structure of the starting material is thought to be related to achieve such a high specific surface area of the products.

Journal Article↗
PubMed2006

Synthesis and electrorheological behavior of sterically stabilized polypyrrole-silica-methylcellulose nanocomposite suspension.

Various polypyrrole (PPy)-silica-methylcellulose nanocomposite particles were synthesized by suspension polymerization in the presence of silica nanoparticles controlling the ratio of pyrrole, silica, and methylcellulose during the polymerization. The electrorheological (ER) and dielectric properties of the sterically stabilized PPy-silica-methylcellulose nanocomposite suspensions were investigated. The ER response increases with the increase in the silica/pyrrole ratio. The ER behavior also depends on the methylcellulose amount during the polymerization. The yield stress initially increases with the methylcellulose amount, passes through a maximum, and then decreases with the methylcellulose amount. The dielectric constants and dc conductivities of the PPy-silica-methylcellulose nanocomposite particles and the dielectric properties of their suspensions indicate that the increased ER response arises from the enhanced interfacial and particle polarization which depends on the silica/pyrrole ratio and the methylcellulose amount during the polymerization.

Journal Article↗
PubMed2006

Probing colloidal forces between a Si3N4 AFM tip and single nanoparticles of silica and alumina.

The atomic force microscope (AFM) has been used to measure surface forces between silicon nitride AFM tips and individual nanoparticles deposited on substrates in 10(-4) and 10(-2) M KCl solutions. Silica nanoparticles (10 nm diameter) were deposited on an alumina substrate and alumina particles (5 to 80 nm diameter) were deposited on a mica substrate using aqueous suspensions. Ionic concentrations and pH were used to manage attractive substrate-particle electrostatic forces. The AFM tip was located on deposited nanoparticles using an operator controlled offset to achieve stepwise tip movements. Nanoparticles were found to have a negligible effect on long-range tip-substrate interactions, however, the forces between the tip and nanoparticle were detectable at small separations. Exponentially increasing short-range repulsive forces, attributed to the hydration forces, were observed for silica nanoparticles. The effective range of hydration forces was found to be 2-3 nm with the decay length of 0.8-1.3 nm. These parameters are in a good agreement with the results reported for macroscopic surfaces of silica obtained using the surface force apparatus suggesting that hydration forces for the silica nanoparticles are similar to those for flat silica surfaces. Hydration forces were not observed for either alumina substrates or alumina nanoparticles in both 10(-4) M KCl solution at pH 6.5 and 10(-2) M KCl at pH 10.2. Instead, strong attractive forces between the silicon nitride tip and the alumina (nanoparticles and substrate) were observed.

Journal Article↗
PubMed2006

Effect of surface interaction of silica nanoparticles modified by silane coupling agents on viscosity of methylethylketone suspension.

In order to control the viscosity of a dense silica methylethylketone (MEK) suspension, the surfaces of silica nanoparticles were modified by 3-glycidoxypropyltrimethoxysilane (GPS) or hexyltrimethoxysilane (C6S) in MEK with the addition of a small amount of pH-controlled water. First, the effect of water addition on the amount of chemisorbed coupling agent was investigated. pH-controlled water enhanced the reactivity of the coupling agent in MEK. The amount of chemisorbed coupling agent increased slightly with the addition of pH 3 water and increased remarkably with the addition of pH 12 water. Next, the effect of the organic functional groups of the coupling agent, pH of the additive water, and additive amount of coupling agent on surface interaction were determined by colloid probe AFM. The steric repulsive force between the silica nanoparticles increased due to water addition, particularly when the pH was maintained at 3. The viscosity of the silica MEK suspension reduced effectively when this repulsive force appeared; however, the optimum condition for reducing the suspension viscosity was dependent on the coupling agent species. The viscosity of the dense silica MEK suspension can be controlled by the addition of small amounts of pH-controlled water and the functional groups of the coupling agent.

Butanones↗
PubMed2006

A two-step route to synthesis of small-pored and thick-walled SBA-16-type mesoporous silica under mildly acidic conditions.

Highly ordered SBA-16-type mesoporous silica materials were synthesized by using poly(ethylene oxide-b-propylene oxide-b-ethylene oxide) triblock copolymer (EO(132)-PO(50)-EO(132), Pluronic F108) as template through a two-step pathway under mildly acidic conditions (pH 2.15-4.50). The highly ordered cage-like mesoporosity of the prepared SBA-16-type mesoporous silica materials having Im3m cubic mesostructure was proved by the well-defined X-ray diffraction patterns combined with transmission electron microscopy. Scanning electron microscopy shows a variation from the spherical agglomerations to the randomly shaped ones with an increase of pH value. The nitrogen adsorption-desorption analysis reveals that the prepared SBA-16-type mesoporous silica materials have a uniform small-sized pore diameter (3.37-4.24 nm) and very thick pore wall (8.84-10.2 nm). These features may make the SBA-16-type mesoporous silica materials synthesized in this study favor the incorporation of catalytically active heteroatoms in silica frameworks, and the functionalization of organic groups for applications in catalysis, sensor and separation. The two-step synthetic method under the mildly acidic conditions can also be extended to the production in the industrial scale as an environmentally friendly way.

Journal Article↗
PubMed2006

Evaluation of five dental silanes on bonding a luting cement onto silica-coated titanium.

OBJECTIVES: Five commercial dental silanes were evaluated in vitro as adhesion promoters bonding a luting cement to silica-coated titanium surfaces. METHODS: Titanium slides (n=20) were cleaned with alumina sand and then silica-coated with a special sand consisting of alumina particles coated with silica. The bonding of a resin composite cement (3M ESPE, Seefeld, Germany) to silica-coated and silanized titanium was evaluated by using the dental silane (RelyX Ceramic Primer) that belongs to the RelyX ARC cementing kit, and comparing it to four other dental silanes (Bisco Porcelain Primer, Cimara, ESPE Sil, and Pulpdent Silane Bond Enhancer). The resin composite cement stubs (n=8) were light-polymerized onto a silanized silica-coated titanium surface. The shear bond strength of the cement stubs was measured after dry storage and thermo-cycling 6000 times between 5 and 55 degrees C. The silanes and their reactions were chemically monitored by using Fourier transform infrared analysis. RESULTS: Statistical analysis using ANOVA revealed that the brand of silanes and the types of storage condition differ significantly (p<0.005). The highest shear bond strength was obtained with RelyX ceramic silane in dry conditions (19.5+/-4.3 MPa), and after thermo-cycling (16.6+/-3.5 MPa). The lowest results were obtained using Pulpdent Silane Bond Enhancer, in dry conditions (7.8+/-2.2 MPa), and after thermocycling (5.3+/-2.4 MPa). The analysis showed that silanes had different pH values. Some differences were detected between the silanes and their reactions. CONCLUSIONS: Dental silanes provide different bonding strengths and have differences in their pH, solvent system and silane concentration.

Adhesiveness↗
PubMed2006

Reuse of waste silica as adsorbent for metal removal by iron oxide modification.

Silica gel is widely used in research laboratories, especially for the purification of organic compounds. Consequently, waste silica gel is generated in increasing amounts. In this work, waste silica was modified by coating its surface with iron oxide aiming to obtain an effective adsorbent for metal removal from wastewater. In the preparation of the adsorbent, the optimal pretreatment temperature and iron concentration were investigated. The coated waste silica was characterized for BET surface area, pore size, specific pore volume and iron content. Iron oxide-coated waste silica was tested for the adsorption of Pb(II), Cu(II), Cd(II) and Ni(II) from solutions in a batch system. The effect of contact time, pH and salt concentration on metal adsorption was investigated. It was found that the adsorption of metals occurred rapidly and reached equilibrium within 30 min. The pH suitable for metal adsorption was between 6 and 7 and leaching of iron from the coating was observed only at pH 3 or lower. The presence of salt reduced the adsorption efficiency of the adsorbent. The adsorption behavior followed both Langmuir and Freundlich isotherms (25 degrees C). Finally, the efficacy of the adsorbents was investigated using aqueous lab waste where removal efficiencies ranging from 62 to 89% were achieved when the initial metal concentrations ranged from 13 to 42 mg L(-1).

Adsorption↗
PubMed2004

Resistance to silica-induced lung fibrosis in senescent rats: role of alveolar macrophages and tumor necrosis factor-alpha (TNF).

The purpose of the present study was to investigate the effect of aging on silica-induced lung toxicity. In young animals silica induced a significant increase in bronchoalveolar lavage tumor necrosis factor-alpha (TNF), lactate dehydrogenase as well as in cell numbers, which correlate with increased collagen deposition and silicotic nodules formations. In old rats, however, no changes in bronchoalveolar lavage or lung parameters were observed following silica instillation. These in vivo results were also confirmed in vitro, where silica failed to induce TNF release in alveolar macrophages obtained from old animals. This defective response to silica could be explained with defective protein kinase C translocation, due to a reduction in its anchoring protein RACK-1 with aging. Overall, these data indicate that the understanding of the molecular mechanisms undelaying toxicity is crucial to define the influence of age on the toxic response and progression of the disease.

Aging↗