916 resultados para Hanging meniscus rotating disk voltammetry


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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

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The accumulation voltammetry of mercury(II) was investigated at a carbon paste electrode chemically modified with silica gel functionalized with 2,5-dimercapto-1,3,4-thiadiazole (DTTPSG-CPE). The repetitive cyclic voltammogram of mercury(II) solution in the potential range -0.2 to +0.8 V (vs. Ag/AgCl), (0.02 mol L-1 KNO3; nu=20 mV s(-1)) show two peaks one at about 0.0 V and other at 0.31 V. However, the cathodic wave peak, around 0.0 V, is irregular and changes its form in each cycle. This peak at about 0.0 V is the reduction current for mercury(II) accumulated in the DTTPSG-CPE. The anodic wave peak at 0.31 V is well-defined and does not change during the cycles. The resultant material was characterized by cyclic and differential pulse anodic stripping voltammetry performed with the electrode in differents supporting electrolytes. The mercury response was evaluated with respect to pH, electrode composition, preconcentration time, mercury concentration, cleaning solution, possible interferences and other variables. The precision for six determinations (n=6) of 0.05 and 0.20 mg (L)-(1) Hg(II) was 2.8 and 2.2% (relative standard deviation), respectively. The method was satisfactory and used to determine the concentration of mercury(II) in natural waters contaminated by this metal.

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

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Objective To compare the effects of decompressive surgery (DSX), electroacupuncture (EAP), and DSX followed by EAP (DSX + EAP) for the treatment of thoracolumbar intervertebral disk disease (IVDD) in dogs with severe neurologic deficits of > 48 hours' duration.Design Retrospective case series and prospective clinical trial.Animals-40 dogs between 3 and 6 yEAPs old and weighing between 10 and 20 kg (22 and 44 lb) with long-standing (>48 hours) clinical signs of severe neurologic disease attributable to thoracolumbar IVDD.Procedures Thoracolumbar medullar injury was classified on the basis of neurologic signs by use of a scale ranging from 1 (least severe) to 5 (most severe). The DSX dogs (n = 10) were retrospectively selected from those that underwent DSX for the treatment of thoracolumbar IVDD. In addition, 19 dogs received EAP alone and 11 dogs underwent DSX followed by EAP (DSX + EAP). Outcome was considered a clinical success when a dog initially classified as grade 4 or 5 was classified as grade 1 or 2 within 6 months after the end of treatment.Results The proportion of dogs with clinical success was significantly higher for dogs that underwent EAP (15/19) than for dogs that underwent DSX (4/10); the proportion of dogs with clinical success for dogs that underwent DSX + EAP was intermediate (8/11).Conclusions and Clinical Relevance EAP was more effective than DSX for recovery of ambulation and improvement in neurologic deficits in dogs with long-standing severe deficits attributable to thoracolumbar IVDD. (J Am Vet Med Assoc 2010;236:1225-1229)

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Lectins are proteins important in various biological processes such as infection, cell differentiation and metastasis. The Parkia pendula lectin has been crystallized using the hanging-drop vapour diffusion method. X-ray diffraction data were collected using a Rigaku RU300 rotating anode generator and R-AXIS IV diffractometer. The cell parameters for P. pendula lectin are a=93.7 Angstrom b=161.1 Angstrom, c=80.0 Angstrom and space group C222. The maximum resolution was of 2.98 Angstrom. These data showed a R-sym=12.8%.

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The CLSI M100-S19 document has recommended the disuse of vancomycin disks for staphylococci and informed that studies on the action of teicoplanin in disk-diffusion testing should be performed. We describe the comparison of two methods, disk diffusion and broth microdilution, for determining teicoplanin susceptibility in clinical isolates of staphylococci. Overall results showed an aggregation rate of 96.8%; Staphylococcus aureus showed total agreement while S. epidermidis showed 93.8% of agreement. According to these local results, disk diffusion can still be employed to teicoplanin susceptibility determination for staphylococci in our institution.

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The application of disk shaped gold ultramicroelectrode for nitrite determination with and without addition of supporting electrolyte was studied using the differential pulse voltammetric method. The well-defined peak for nitrite oxidation near 0.8V (vs. Ag/AgCl reference electrode) was used to obtain analytical plots in the concentration range from 0.1 to 0.6 mmol L-1 and from 10.0 to 50.0 mu mol.L-1. The calculated detection limit was 0.65 mu mol.L-1 in purified water, in the absence of supporting electrolyte, with relative standard deviation of 1.36% (n=6) for analyzing 10.0 mu mol L-1 nitrite solutions, and accuracy of 100.9 %, based on recovery studies. The application of this analytical method to mineral and river water samples of natural pH also showed improved sensitivity when compared with the linear sweep voltammetric method previously reported.

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The determination of lead ions directly in water, for application in analysis of samples of environmental interest, was studied by electroanalytical techniques. Linear sweep anodic stripping voltammetry with a carbon fiber disk ultramicroelectrode (7.0 mu m in diameter), without mercury film, has been used for lead determination, by standard addition, in purified water in the absence of supporting electrolyte. The response was linear in the range from 10.0 to 50.0 mu g L-1, with a detection limit of 0.8 mu g L-1, for 300 s preconcentration time, at -1.2 V and 1.0 V s(-1) scan rate. The reliability of the analytical procedure was evaluated by precision using relative standard deviations (5.6%, for three repetitive stripping current measurements of solution with 10.0 mu g L-1 lead ions) and by the accuracy with recovery experiments (mean of 110.8%) for the same concentration.

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Solid paraffin-based carbon paste electrodes modified with 2-aminothiazole organofunctionalized silica have been applied to the anodic stripping determination of copper ions in ethanol fuel samples without any sample treatment. The proposed method comprised four steps: (1) copper ions preconcentration at open circuit potential directly in the ethanol fuel sample; (2) exchange of the solution and immediate cathodic reduction of the absorbate at controlled potential; (3) differential pulse anodic stripping voltammetry; (4) electrochemical surface regeneration by applying a positive potential in acid media. Factors affecting the preconcentration, reduction and stripping steps were investigated and the optimum conditions were employed to develop the analytical procedure. Using a preconcentration time of 20 min and reduction time of 120 s at -0.3 V versus Ag/AgCl(sat) a linear range from 7.5 x 10(-8) to 2.5 x 10(-6) mol L(-1) with detection limit of 3.1 x 10(-8) mol L(-1) was obtained. Interference studies have shown a decrease in the interference effect according to the sequence: Ni > Zn > Cd > Pb > Fe. However, the interference effects of these ions have not forbidden the application of the proposed method. Recovery values between 98.8 and 102.3% were obtained for synthetic samples spiked with known amounts of Cu(2+) and interfering metallic ions. The developed electrode was successfully applied to the determination of Cu(2+) in commercial ethanol fuel samples. The results were compared to those obtained by flame atomic absorption spectroscopy by using the F-test and t-test. Neither F-value nor t-value have exceeded the critical values at 95% confidence level, confirming that there are no significant differences between the results obtained by both methods. (c) 2006 Elsevier B.V. All rights reserved.

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

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Lys49-Phospholipase A(2) (Lys49-PLA(2) - EC 3.1.1.4) homologues damage membranes by a Ca2+-independent mechanism which does not involve catalytic activity. Both MjTX-II from Bothrops moojeni and BthTX-I from Bothrops jararacussu are dimeric in solution and in the crystalline states, and a model for the Ca2+-independent membrane damaging mechanism has been suggested in which flexibility at the dimer interface region pert-nits quaternary structural transitions between open and closed membrane bound dimer conformations which results in the perturbation of membrane phospholipids and disruption of the bilayer structure [1]. With the aim of gaining insights into the structural determinants involved in protein/lipid association, we report here the crystallization and preliminary X-ray analysis of the (i) MjTX-II/SDS complex at a resolution of 2.78Angstrom, (ii) MjTX-II/STE complex at a resolution of 1.8 Angstrom and (W) BthTX-I/DMPC complex at 2.72Angstrom. These complexes were crystallized by the hanging drop vapour-diffusion technique in (i) HEPES buffer (pH 7.5) 1.8M ammonium sulfate with 2% (w/v) polyethyleneglycol 400, in (ii) 0.6-0.8 M sodium citrate as the precipitant (pH 6.0-6.5) and in (iii) sodium citrate buffer (pH 5.8) and PEG 4000 and 20% isopropanol, respectively. Single crystals of these complexes have been obtained and X-ray diffraction data have been collected at room temperature using a R-AXIS IV imaging plate system and graphite monochromated Cu Kalpha X-ray radiation generated by a Rigaku RU300 rotating anode generator for (i) and (W) and using using a Synchrotron Radiation Source (Laboratorio Nacional de Luz Sincrotron, LNLS, Campinas, Brazil) for (ii).

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This study evaluated the effect of different thickness of disk-shaped specimens on the push-out bond strength test. Eighteen lower bovine teeth were sectioned (20mm) and prepared (15mm) with the same post system drill (Light Post (R) #1, Schaumburg, IL, Bisco, USA). The apical third of each specimen was embedded in a plastic matrix filled with an acrylic resin (Dencrilay (TM), Dencril, São Paulo, Brazil). The posts were cleaned with alcohol, silanated (ProSil (R), FGM, Joenville, SC, Brazil) and cemented with the RelyX (TM) U100 (3M ESPE, St. Paul, MN, USA). Each specimen was sectioned into three pieces of differing thicknesses (1, 2, and 4 mm). These disk-samples were allocated into 3 groups (n=18) and subjected to push-out testing. One-way ANOVA showed no influence of the specimen thickness on the results (p=0.842). No correlation was observed between thickness and push-out bond strength (Pearson Correlation, r(2)=0.0688; P=0.6209). The push-out bond strength test was not affected by the thickness of the disk-specimens.

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We consider an electric charge, minimally coupled to the Maxwell field, rotating around a Schwarzschild black hole. We investigate how much of the radiation emitted from the swirling charge is absorbed by the black hole and show that most of the photons escape to infinity. For this purpose we use the Gupta-Bleuler quantization of the electromagnetic field in the modified Feynman gauge developed in the context of quantum field theory in Schwarzschild spacetime. We obtain that the two photon polarizations contribute quite differently to the emitted power. In addition, we discuss the accurateness of the results obtained in a full general relativistic approach in comparison with the ones obtained when the electric charge is assumed to be orbiting a massive object due to a Newtonian force.

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The effects of a sudden increase and decrease of the interatomic interaction and harmonic-oscillator trapping potential on vortices in a quasi two-dimensional rotating Bose-Einstein condensate are investigated using the mean-field Gross-Pitaevskii equation. We also study the decay of vortices when the rotation of the condensate is suddenly stopped. Upon a free expansion of a rotating BEC with vortices the radius of the vortex core increases more rapidly than the radius of the condensate. (C) 2002 Elsevier B.V. B.V. All rights reserved.