949 resultados para THIN-LAYER-CHROMATOGRAPHY


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The aim of this work was to describe the morphology and ontogeny of P. riedelii fruits to aid in taxonomic, ecological and phylogenetic studies in Apocynaceae. Fruits were fixed in FAA, embedded in plastic resin, sectioned at 10 ìm and stained with toluidine blue, for structural analysis. The fruit of P. riedelii is a follicarium, with two follicular fruitlets. The epicarp is one-cell-layered, with trichomes and thick cuticle. The mesocarp, originating from fundamental ovary tissue, is parenchymatous with laticifers, non-lignified fibers and vascular bundles. The endocarp sensu lato is two-celllayered of crossed sclereids, originating from the inner ovary epidermis and from a single layer of parenchyma cells of fundamental ovary tissue. Follicle dehiscence is lateral and the dehiscence process involves anatomical characteristics such as a dehiscence zone with thin-walled cells, non-lignified fibers in the mesocarp and crossed sclereids in the endocarp.

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This study analyzed the reaction layer and measured the marginal crown fit of cast titanium applied to different phosphate-bonded investments, prepared under the following conditions (liquid concentration/casting temperature): Rema Exakt (RE) - 100%/237°C, 75%/287°C, Castorit Super C (CS)-100%/70°C, 75%/141°C and Rematitan Plus (RP)- 100%/430°C (special to titanium cast, as the control group). The reaction layer was studied using the Vickers hardness test, and analyzed by two way ANOVA and Tukey's HSD tests (α = 0.05). Digital photographs were taken of the crowns seated on the die, the misfit was measured using an image analysis system and One-way ANOVA, and Tukey's test was applied (α = 0.05). The hardness decreased from the surface (601.17 VHN) to 150 μm (204.03 VHN). The group CS 75%/141°C presented higher hardness than the other groups, revealing higher surface contamination, but there were no differences among the groups at measurements deeper than 150 μm. The castings made with CS - 100%/70°C presented the lowest levels of marginal misfit, followed by RE -100%/237°C. The conventional investments CS (100%) and RE (100%) showed better marginal fit than RP, but the CS (75%) had higher surface contamination.

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PURPOSE: In this case report, the clinical performance of a microhybrid resin composite placed with or without a flowable resin composite was compared, over a 48-month period. CASE DESCRIPTION: The patient of this case report presented 2 pairs of equivalent cervical abfraction lesions, under occlusion. Four restorations were placed in teeth 34, 35, 44 and 45. The restorations were divided into groups (Single Bond + Filtek-Flow + Filtek Z250 or Single Bond + Filtek Z250) and the materials were applied according to the manufactures instructions. Two previously calibrated operators placed the restorations and two other independent examiners evaluated the restorations at baseline and after 48 months, according to the USPHS criteria and modified criteria for color match. CONCLUSION: After 48 months of evaluation the lesions restored with Filtek-Flow as a liner under Filtek Z250 did not show better clinical performance than the restorations without Filtek-Flow. All restorations showed a trend toward dark yellowing after 48 months.

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The General Ocean Turbulence Model (GOTM) is applied to the diagnostic turbulence field of the mixing layer (ML) over the equatorial region of the Atlantic Ocean. Two situations were investigated: rainy and dry seasons, defined, respectively, by the presence of the intertropical convergence zone and by its northward displacement. Simulations were carried out using data from a PIRATA buoy located on the equator at 23º W to compute surface turbulent fluxes and from the NASA/GEWEX Surface Radiation Budget Project to close the surface radiation balance. A data assimilation scheme was used as a surrogate for the physical effects not present in the one-dimensional model. In the rainy season, results show that the ML is shallower due to the weaker surface stress and stronger stable stratification; the maximum ML depth reached during this season is around 15 m, with an averaged diurnal variation of 7 m depth. In the dry season, the stronger surface stress and the enhanced surface heat balance components enable higher mechanical production of turbulent kinetic energy and, at night, the buoyancy acts also enhancing turbulence in the first meters of depth, characterizing a deeper ML, reaching around 60 m and presenting an average diurnal variation of 30 m.

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Mixing layers are present in very different types of physical situations such as atmospheric flows, aerodynamics and combustion. It is, therefore, a well researched subject, but there are aspects that require further studies. Here the instability of two-and three-dimensional perturbations in the compressible mixing layer was investigated by numerical simulations. In the numerical code, the derivatives were discretized using high-order compact finite-difference schemes. A stretching in the normal direction was implemented with both the objective of reducing the sound waves generated by the shear region and improving the resolution near the center. The compact schemes were modified to work with non-uniform grids. Numerical tests started with an analysis of the growth rate in the linear regime to verify the code implementation. Tests were also performed in the non-linear regime and it was possible to reproduce the vortex roll-up and pairing, both in two-and three-dimensional situations. Amplification rate analysis was also performed for the secondary instability of this flow. It was found that, for essentially incompressible flow, maximum growth rates occurred for a spanwise wavelength of approximately 2/3 of the streamwise spacing of the vortices. The result demonstrated the applicability of the theory developed by Pierrehumbet and Widnall. Compressibility effects were then considered and the maximum growth rates obtained for relatively high Mach numbers (typically under 0.8) were also presented.

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The flavonoids present in sugarcane (Saccharum officinarum) extracts were analyzed by liquid chromatography - mass spectrometry (LC-MS), and a study of the fragmentation patterns of selected flavonoids was conducted using orthogonal acceleration time-of-flight electrospray ionization mass spectrometry (ESI-oa-ToF MS). Seven C- and O-glycosylflavones were identified in the extracts, namely, schaftoside, isoschaftoside, luteolin-8-C-(rhamnosylglucoside), vitexin, orientin, tricin-7-O-neohesperidoside and tricin-7-O-glucoside. Of these, five were identified in the absence of direct comparison with their respective standards. The described method also permitted the differentiation of the 6-C and 8-C isomeric flavones, schaftoside and isoschaftoside. The combination of fragmentation data and exact mass measurement showed to be complimentary to the HPLC-UV-MS techniques previously utilized for isomers discrimination in sugarcane studies.

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This paper describes a sequential injection chromatography procedure for determination of picloram in waters exploring the low backpressure of a 2.5 cm long monolithic C18 column. Separation of the analyte from the matrix was achieved in less than 60 s using a mobile phase composed by 20:80 (v v-1) acetonitrile:5.0 mmol L-1 H3PO4 and flow rate of 30 μL s-1. Detection was made at 223 nm with a 40 mm optical path length cell. The limits of detection and quantification were 33 and 137 μg L-1, respectively. The proposed method is sensitive enough to monitor the maximum concentration level for picloram in drinking water (500 μg L-1). The sampling frequency is 60 analyses per hour, consuming only 300 μL of acetonitrile per analysis. The proposed methodology was applied to spiked river water samples and no statistically significant differences were observed in comparison to a conventional HPLC-UV method.

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A new tetraruthenated copper(II)-tetra(3,4-pyridyl)porphyrazine species, [CuTRPyPz]4+, has been synthesized and fully characterized by means of analytical, spectroscopic and electrochemical techniques. This À-conjugated system contrasts with the related meso-tetrapyridylporphyrins by exhibiting strong electronic interaction between the coordinated peripheral complexes and the central ring. Based on favorable À-stacking and electrostatic interactions, layer-by-layer assembled films were successfully generated from the appropriate combination of [CuTRPyPz]4+ with copper(II)-tetrasulfonated phtalocyanine, [CuTSPc]4-. Their conducting and electrocatalytic properties were investigated by means of impedance spectroscopy and rotating disc voltammetry, exhibiting metallic behavior near the Ru(III/II) redox potential, as well as enhanced catalytic activity for the oxidation of nitrite and sulphite ions.

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Colloidal particles have been used to template the electrosynthesis of several materials, such as semiconductors, metals and alloys. The method allows good control over the thickness of the resulting material by choosing the appropriate charge applied to the system, and it is able to produce high density deposited materials without shrinkage. These materials are a true model of the template structure and, due to the high surface areas obtained, are very promising for use in electrochemical applications. In the present work, the assembly of monodisperse polystyrene templates was conduced over gold, platinum and glassy carbon substrates in order to show the electrodeposition of an oxide, a conducting polymer and a hybrid inorganic-organic material with applications in the supercapacitor and sensor fields. The performances of the resulting nanostructured films have been compared with the analogue bulk material and the results achieved are depicted in this paper.

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We describe the concept, the fabrication, and the most relevant properties of a piezoelectric-polymer system: Two fluoroethylenepropylene (FEP) films with good electret properties are laminated around a specifically designed and prepared polytetrafluoroethylene (PTFE) template at 300 degrees C. After removing the PTFE template, a two-layer FEP film with open tubular channels is obtained. For electric charging, the two-layer FEP system is subjected to a high electric field. The resulting dielectric barrier discharges inside the tubular channels yield a ferroelectret with high piezoelectricity. d(33) coefficients of up to 160 pC/N have already been achieved on the ferroelectret films. After charging at suitable elevated temperatures, the piezoelectricity is stable at temperatures of at least 130 degrees C. Advantages of the transducer films include ease of fabrication at laboratory or industrial scales, a wide range of possible geometrical and processing parameters, straightforward control of the uniformity of the polymer system, flexibility, and versatility of the soft ferroelectrets, and a large potential for device applications e.g., in the areas of biomedicine, communications, production engineering, sensor systems, environmental monitoring, etc.

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In some circumstances ice floes may be modeled as beams. In general this modeling supposes constant thickness, which contradicts field observations. Action of currents, wind and the sequence of contacts, causes thickness to vary. Here this effect is taken into consideration on the modeling of the behavior of ice hitting inclined walls of offshore platforms. For this purpose, the boundary value problem is first equated. The set of equations so obtained is then transformed into a system of equations, that is then solved numerically. For this sake an implicit solution is developed, using a shooting method, with the accompanying Jacobian. In-plane coupling and the dependency of the boundary terms on deformation, make the problem non-linear and the development particular. Deformation and internal resultants are then computed for harmonic forms of beam profile. Forms of giving some additional generality to the problem are discussed.

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Metal oxide-semiconductor capacitors with TiO(x) deposited with different O(2) partial pressures (30%, 35%, and 40%) and annealed at 550, 750, and 1000 degrees C were fabricated and characterized. Fourier transform infrared, x-ray near edge spectroscopy, and elipsometry measurements were performed to characterize the TiO(x) films. TiO(x)N(y) films were also obtained by adding nitrogen to the gaseous mixture and physical results were presented. Capacitance-voltage (1 MHz) and current-voltage measurements were utilized to obtain the effective dielectric constant, effective oxide thickness, leakage current density, and interface quality. The results show that the obtained TiO(x) films present a dielectric constant varying from 40 to 170 and a leakage current density (for V(G)=-1 V, for some structures as low as 1 nA/cm(2), acceptable for complementary metal oxide semiconductor circuits fabrication), indicating that this material is a viable, in terms of leakage current density, highk substitute for current ultrathin dielectric layers. (C) 2009 American Vacuum Society. [DOI: 10.1116/1.3043537]

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In this work, we investigate the interplay between surface anchoring and finite-size effects on the smectic-isotropic transition in free-standing smectic films. Using an extended McMillan model, we study how a homeotropic anchoring stabilizes the smectic order above the bulk transition temperature. In particular, we determine how the transition temperature depends on the surface ordering and film thickness. We identify a characteristic anchoring for which the transition temperature does not depend on the film thickness. For strong surface ordering, we found that the thickness dependence of the transition temperature can be well represented by a power-law relation. The power-law exponent exhibits a weak dependence on the range of film thicknesses, as well as on the molecular alkyl tail length. Our results reproduce the main experimental findings concerning the layer-thinning transitions in free-standing smectic films.

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Objective: To describe the ultrastructure of the interface between periodontal tissues and titanium mini-implants in rat mandibles. Materials and Methods: A titanium mini-implant was placed between the buccal roots of the mandibular first molar of 24 adult rats. After 21, 30, 45, 60, 90, and 120 days of implantation, the mandibular portion was removed and fixed in cacodylate-buffered 2% glutaraldehyde + 2.5% formaldehyde. The material was decalcified and processed for scanning and transmission electron microscopy. Results: Ultrastructural analysis revealed a thin cementum-like layer at longer times after implantation at the areas in which the periodontal ligament was in contact with the implant. Conclusions: The alveolar bone and the periodontal ligament reorganized their constituents around the implant, and a thin cementum-like layer was formed at longer times after implantation at the areas in which the periodontal ligament was in contact with the implant. (Angle Orthod. 2010;80:459-435.)

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Background: The thin-spined porcupine, also known as the bristle-spined rat, Chaetomys subspinosus (Olfers, 1818), the only member of its genus, figures among Brazilian endangered species. In addition to being threatened, it is poorly known, and even its taxonomic status at the family level has long been controversial. The genus Chaetomys was originally regarded as a porcupine in the family Erethizontidae, but some authors classified it as a spiny-rat in the family Echimyidae. Although the dispute seems to be settled in favor of the erethizontid advocates, further discussion of its affinities should be based on a phylogenetic framework. In the present study, we used nucleotide-sequence data from the complete mitochondrial cytochrome b gene and karyotypic information to address this issue. Our molecular analyses included one individual of Chaetomys subspinosus from the state of Bahia in northeastern Brazil, and other hystricognaths. Results: All topologies recovered in our molecular phylogenetic analyses strongly supported Chaetomys subspinosus as a sister clade of the erethizontids. Cytogenetically, Chaetomys subspinosus showed 2n = 52 and FN = 76. Although the sexual pair could not be identified, we assumed that the X chromosome is biarmed. The karyotype included 13 large to medium metacentric and submetacentric chromosome pairs, one small subtelocentric pair, and 12 small acrocentric pairs. The subtelocentric pair 14 had a terminal secondary constriction in the short arm, corresponding to the nucleolar organizer region (Ag-NOR), similar to the erethizontid Sphiggurus villosus, 2n = 42 and FN = 76, and different from the echimyids, in which the secondary constriction is interstitial. Conclusion: Both molecular phylogenies and karyotypical evidence indicated that Chaetomys is closely related to the Erethizontidae rather than to the Echimyidae, although in a basal position relative to the rest of the Erethizontidae. The high levels of molecular and morphological divergence suggest that Chaetomys belongs to an early radiation of the Erethizontidae that may have occurred in the Early Miocene, and should be assigned to its own subfamily, the Chaetomyinae.