Molecularly imprinted silica films prepared by electroassisted deposition for the selective detection of dopamine

Dopamine (DA) can be detected by electrochemical oxidation in conventional electrodes. However, the presence of other oxidizable species (interferents) usually present in physiological fluids at high concentrations (like ascorbic acid) makes very difficult its electrochemical detection. In the present work, glassy carbon electrodes have been modified with molecularly imprinted silica (MIS) films prepared by electroassisted deposition of sol–gel precursors. The production of MIS films was performed by adding the template molecule (DA) to the precursor sol. The molecular impression of silica was assessed showing a high coherency allowing a filtering capacity in the molecular scale. The MIS-modified electrodes present a high selectivity for the detection of DA in neutral or acidic solutions. The MIS-modified electrodes allow the amperometric determination of dopamine in solutions containing ascorbic acid with molar ratios lower than 1:50,000.

Tailored mesoporous silica supports for Ni catalysed hydrogen production from ethanol steam reforming

Mesoporous silica supported Ni nanoparticles have been investigated for hydrogen production from ethanol steam reforming. Ethanol reforming is structure-sensitive over Ni, and also dependent on support mesostructure; three-dimensional KIT-6 possessing interconnected mesopores offers superior metal dispersion, steam reforming activity, and on-stream stability against deactivation compared with a two-dimensional SBA-15 support.

Grafting of adipic anhydride to carbon nanotubes through a Diels-Alder cycloaddition/oxidation cascade reaction

Accepted Manuscript

Estudo comparativo entre sílica obtida por lixívia ácida da casca de arroz e sílica obtida por tratamento térmico da cinza de casca de arroz

A comparison between silica by acid leaching of rice husk (RH) and silica obtained from thermal treatment of rice husk ash (RHA) is presented. The best leaching results were obtained using 10% hydrochloric acid followed by washing with water. The alternative method, calcination of RHA at 700 ºC for 6 h followed by grinding for 80 min, was more effective. Silica obtained from RH was about 97% amorphous, had a 17.37 µm mean particle size, and a specific surface area of 296 m²/g. On the other hand, for silica obtained from RHA the values were about 95% amorphous material 0.68 µm, and 81 m²/g.

Síntese, caracterização e estudo da regeneração do silicoaluminofosfato-11 (SAPO-11)

heterogeneous catalyst such as a silicoaluminophosphate, molecular sieve with AEL (Aluminophosphate eleven) structure such as SAPO-11, was synthesized through the hydrothermal method starting from silica, pseudoboehmite, orthophosphoric acid (85%) and water, in the presence of a di-isopropylamine organic template. For the preparation of SAPO-11 in a dry basis it was used as reactants: DIPA; H3PO4; SiO4; Pseudoboehmite and distilled water. The crystallization process occurred when the reactive hydrogel was charged into a vessel and autoclaved at 200ºC for a period of 72 hours under autogeneous pressure. The obtained material was washed, dried and calcined to remove the molecular sieves of DIPA. The samples were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), infrared spectroscopy (FT-IR), nitrogen adsorption (BET) and thermal analysis (TG/DTG). The acidic properties were determined using adsorption of nbutylamine followed by programmed thermodessorption. This method revealed that SAPO-11 shows an acidity that ranges from weak to moderate. However, a small quantity of strong acid sites could be detected there. The deactivation of the catalysts was conducted by artificial coking followed by the cracking of the n-hexane in a fixed bed with a continuous flow micro-reactor coupled on line to a gas chromatograph. The main products obtained were: ethane, propane, isobutene, n-butane, n-pentane and isopentane. The Vyazovkin (model-free) kinetics method was used to determine the regeneration and removal of the coke

Effect of surface conditioning methods on the microtensile bond strength of resin composite to composite after aging conditions

Objectives. This study evaluated the effect of two different surface conditioning methods on the repair bond strength of a bis-GMA-adduct/bis-EMA/TEGDMA based resin composite after three aging conditions.Methods. Thirty-six composite resin blocks (Esthet X, Dentsply) were prepared (5 mm x 6 mm x 6 mm) and randomly assigned into three groups for aging process: (a) immersion in citric acid (pH 3.0 at 37 degrees C, 1 week) (CA); (b) boiling in water for 8h (BW) and (c) thermocycling (x5000, 5-55 degrees C, dwell time: 30s) (TC). After aging, the blocks were assigned to one of the following surface conditioning methods: (1) silica coating (30 mu m SiOx) (CoJet, 3M ESPE) + silane (ESPE-Sil) (CJ), (2) phosphoric acid + adhesive resin (Single Bond, 3M ESPE) (PA). Resin composite (Esthet.X (R)) was bonded to the conditioned substrates incrementally and light polymerized. The experimental groups formed were as follows: Gr1:CA + PA; Gr2:CA + CJ Gr3:BW + PA; Gr4: BW + CJ; Gr5:TC + PA; Gr6: TC + CJ. The specimens were sectioned in two axes (x and y) with a diamond disc under coolant irrigation in order to obtain non-trimmed bar specimens (sticks, 10 mm x 1 mm x 1 mm) with 1 mm(2) of bonding area. The microtensile test was accomplished in a universal testing machine (crosshead speed: 0.5 mm min(-1)).Results. The means and standard deviations of bond strength (MPa +/- S.D.) per group were as follows: Gr1: 25.5 +/- 10.3; Gr2: 46.3 +/- 10.1; Gr3: 21.7 +/- 7.1; Gr4: 52.3 +/- 15.1; GrS: 16.1 +/- 5.1; Gr6, 49.6 +/- 13.5. The silica coated groups showed significantly higher mean bond values after all three aging conditions (p < 0.0001) (two-way ANOVA and Tukey tests, alpha = 0.05). The interaction effect revealed significant influence of TC aging on both silica coated and acid etched groups compared to the other aging methods (p < 0.032). Citric acid was the least aggressive aging medium.Significance. Chairside silica coating and silanization provided higher resin-resin bond strength values compared to acid etching with phosphoric acid followed by adhesive resin applications. Thermocycling the composite substrates resulted in the lowest repair bond strength compared to citric acid challenge or boiling in water. (C) 2006 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Bond strength durability of direct and indirect composite systems following surface conditioning for repair

Purpose: This study evaluated the effect of surface conditioning methods and thermocycling on the bond strength between a resin composite and an indirect composite system in order to test the repair bond strength. Materials and Methods: Eighteen blocks (5 x 5 x 4 mm) of indirect resin composite (Sinfony) were fabricated according to the manufacturer's instructions. The specimens were randomly assigned to one of the following two treatment conditions (9 blocks per treatment): (1) 10% hydrofluoric acid (HF) for 90 s (Dentsply) + silanization, (2) silica coating with 30-Ìm SiOx particles (CoJet) + silanization. After surface conditioning, the bonding agent was applied (Adper Single Bond) and light polymerized. The composite resin (W3D Master) was condensed and polymerized incrementally to form a block. Following storage in distilled water at 37°C for 24 h, the indirect composite/resin blocks were sectioned in two axes (x and y) with a diamond disk under coolant irrigation to obtain nontrimmed specimens (sticks) with approximately 0.6 mm2 of bonding area. Twelve specimens were obtained per block (N = 216, n = 108 sticks). The specimens from each repaired block were again randomly divided into 2 groups and tested either after storage in water for 24 h or thermocycling (6000 cycles, 5°C to 55°C). The microtensile bond strength test was performed in a universal testing machine (crosshead speed: 1 mm/min). The mean bond strengths of the specimens of each block were statistically analyzed using two-way ANOVA (α = 0.05). Results: Both surface conditioning (p = 0.0001) and storage conditions (p = 0.0001) had a significant effect on the results. After 24 h water storage, silica coating and silanization (method 2) showed significantly higher bond strength results (46.4 ± 13.8 MPa) than that of hydrofluoric acid etching and silanization (method 1) (35.8 ± 9.7 MPa) (p < 0.001). After thermocycling, no significant difference was found between the mean bond strengths obtained with method 1 (34.1 ± 8.9 MPa) and method 2 (31.9 ± 7.9 MPa) (p > 0.05). Conclusion: Although after 24 h of testing, silica coating and silanization performed significantly better in resin-resin repair bond strength, both HF acid gel and silica coating followed by silanization revealed comparable bond strength results after thermocycling for 6000 times.

Fatigue resistance of bovine teeth restored with resin-bonded fiber posts: Effect of post surface conditioning

This study evaluated the effect of post surface conditioning on the fatigue resistance of bovine teeth restored with resin-bonded fiber-reinforced composite (FRC). Root canals of 20 single-rooted bovine teeth (16 mm long) were prepared to 12 mm using a preparation drill of a double-tapered fiber post system. Using acrylic resin, each specimen was embedded (up to 3.0 mm from the cervical part of the specimen) in a PVC cylinder and allocated into one of two groups (n = 10) based on the post surface conditioning method: acid etching plus silanization or tribochemical silica coating (30 μm SiOx + silanization). The root canal dentin was etched (H2PO3 for 30 seconds), rinsed, and dried. A multi-step adhesive system was applied to the root dentin and the fiber posts were cemented with resin cement. The specimens were submitted to one million fatigue cycles. After fatigue testing, a score was given based on the number of fatigue cycles until fracture. All of the specimens were resistant to fatigue. No fracture of the root or the post and no loss of retention of the post were observed. The methodology and the results of this study indicate that tribochemical silica coating and acid etching performed equally well when dynamic mechanical loading was used.

Preparação e caracterização de sílicas mesoporosas

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Preparação e caracterização estrutural de aerogéis de sílica com diferentes concentrações de F127

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Estudo da passagem de diferentes concentrações de ácido fosfórico através da dentina e observação da morfologia dentinária pelo microscópio eletrônico de varredura

Pós-graduação em Odontologia Restauradora - ICT

A chemical approach to Heusler compounds and nanoparticles

Heusler Materialien wurden bisher vor allem in Volumen- und Dünnfilmproben aufgrund ihrer technischen Bedeutung untersucht. In dieser Arbeit berichtet über die experimentellen Untersuchungen der chemischen Synthese, Struktur, und der magnetischen Eigenschaften von ternären Heusler-Nanopartikeln. Die grundlegenden Aspekte der Physik, Chemie und Materialwissenschaft bezüglich der Heusler Nanopartiikel wurden untersucht. Außerdem wurde eine silicatgestützte Herstellungsmethode für Karbon-ummantelte, ternäre intermetallische Co2FeGa Nanopartikel entwickelt. Die Bildung der L21 Co2FeGa Phase wurde mit Röntgenbeugung (XRD), Extended X-ray Absorption Fine Structure Spektroskopie (EXAFS), und 57Fe Mössbauer Spektroskopie bestätigt. Die Abhängigkeit der Phase und der der Größe der Co2FeGa Nanopartikel vom der Zusammensetzung der Precursor und des Silicats wurden untersucht. Durch das Koppeln der aus Transmissions-Elektronen-Mikroskopie (TEM) gewonnen Teilchengröße und der Mössbauerspektroskopie konnte die kritische Größe für den Übergang von superparamgnetischem zu ferromagnetischem Verhalten von Co2FeGa Nanopartikel ermittelt werden. Die silicatgestützte chemische Synthese von Co2FeGa Nanopartikeln besitzt großes Potential für eine generelle Herstellungsmethode für Co-basierte Heuser Nanopartikel. Des weiteren wurde auch eine chemische Herstellungsmethode von metallischen Nanopartikeln mit Synchrotronstrahlung untersucht, die so gewonnen Nanopartikel sind vielversprechende Materialien für die Nanobiotechnologie und die Nanomedizin.

Geochemistry of some manganese nodules

The manganese nodules occur in greater or less quantity all over the ocean-bed, and most abundantly in the Pacific. They occur in all sizes, from minute grains to masses of a pound weight, and even greater, and form nodular concretions of concentric shells, round a nucleus, which is very frequently a piece of pumice or a shark's tooth. Their outside has a peculiar and very characteristic mammillated surface, which enables them to be identified at a glance. When freshly brought up they are very soft, being easily scraped to powder with a knife. They gradually get harder on exposure to the air. The powder, heated in a closed tube, gives out water which re-acts alkaline, and has an empyreumatic odour. Heated with strong hydrochloric acid, it liberates abundance of chlorine, and the residue which remains is white, consisting of silica, clay, and sand, the sand being the same as is found in the bottom mud from the same locality. Their composition varies greatly, different nodules containing different quantities of mechanically admixed mud, and the number of different elements found in them is very large. Copper, iron, cobalt, nickel, manganese, alumina, lime, magnesia, silica, and phosphoric acid have been detected in a large number; but I have not as yet been able to make a complete analysis of any of them. I have, however, made a few determinations of the most important component substances. For this purpose the outside and densest layers of the nodules were selected, and portions of them were pulverised and dried for ten or twelve hours at 140° C. The amount of chlorine liberated on treatment with hydrochloric acid was determined by Bunsen's method, and the iron was determined by titration with stannous chloride. The samples analysed were from four different localities.