108 resultados para Scanning reference electrode technique
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This study evaluated the microleakage of pit and fissure sealants after different surface preparation (invasive technique and laser irradiation) and the use of different materials (fluoride resin-filled sealant, resin-modified glass ionomer cement and adhesive system). Eighty-four pre molars were used in this study, which were divided into seven groups. After the accomplishment of the different treatments, these were submitted to thermocycling process and assess for microleakage by examination under an epifluorescent microscope and scored zero to seven. Two specimens of each group were observed under scanning electron microscope (SEM). The results showed that laser irradiation did not lessen microleakage in pit and fissures when using a filled-resin sealant with fluoride or a resin-modified glass ionomer cement. The use of laser irradiation and adhesive system, followed by a resin-filled sealant with fluoride, showed the lowest microleakage scores in pit and fissures. Comparing this group to the resin-modified glass ionomer cement group, there was statistical significance. The use of a adhesive system decreased microleakage when using a fluoride resin-filled sealant with or without previous laser irradiation; although it was not statistically significant.
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A flow-injection system with a glassy carbon disk electrode modified with Prussian Blue film is proposed for the determination of persulfate in commercial samples of hair bleaching boosters by amperometry. The detection was obtained by chronoamperometric technique and the sample is injected into the electrochemical cell in a wall jet configuration. Potassium chloride at concentration of 0.1 mol L-1 acted as sample carrier at a flow rate of 4.0 mL min-1 and supporting-electrolyte. For 0.025 V (vs. Ag/AgCl) applied voltage, the proposed system handles ca. 160 samples per hour (1.0 10-4 - 1.0 10-3 mol L-1 of persulfate), consuming about 200 μL sample and 11 mg KCl per determination. Typical linear correlations between electrocatalytic current and persulfate concentration was ca. 0.9998. The detection limit is 9.0 10-5 mol L-1 and the calculated amperometric sensibility 3.6 103 μA L mol -1. Relative standard deviation (n =12) of a 1.0 10-4 mol L-1 sample is about 2.2%. The method was applied to persulfate determination in commercial hair-bleaching samples and results are in agreement with those obtained by titrimetry at 95% confidence level and good recoveries (95 - 112%) of spiked samples were found. © 2003 by MDPI.
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The electrochemistry reduction for the removal of Reactive Blue 4 (RB4) dye from aqueous solution using reticulated glassy carbon electrode is investigated. At pH < 8.0 the anthraquinone group of the RB4 dye are reduced in one cathodic step to hidroquinone after a reversible two-electron process involving a precedent two protons reaction. A stable semiquinone is detected by spectrophotometric technique. At pH > 8.0 the reduction process involves two reversible 2-electron steps, whose species are generated by a protonation equilibrium of anthraquinone group. The results shows that 60% of color removal was obtained after 3 hours of RB4 dye electrolysis at acidic and neutral conditions and only 37% at alkaline conditions. Simultaneously 64% of total organic carbon was removed after electrolysis at pH 2.0.
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In this work, electrochemical oxidation of albendazole (ABZ) was carried out using a glassy carbon-rotating disk electrode. Development of electroanalytical methodology for ABZ quantification in pharmaceutical formulations was also proposed by using linear sweep voltammetric technique. Electrochemical oxidation is observed for ABZ at E 1/2 = 0.99:V vs. Ag/AgCl sat, when an anodic wave is observed. Kinetic parameters obtained for ABZ oxidation exhibited a standard heterogeneous rate constant for the electrodic process equal to (1.51 ± 0.07) ± 10 -5:cm:s -1, with a αn a value equal to 0.76. Limiting current dependence against ABZ concentration exhibited linearity on 5.0 ± 10 -5 to 1.0 ± 10 -2:mol:l -1 range, being obtained a detection limit of 2.4 ± 10 -5:mol:l -1. Proposed methodology was applied to ABZ quantification in pharmaceutical formulations. © 2005 Elsevier SAS. All rights reserved.
Resumo:
A mercury-sensitive chemically modified graphite paste electrode was constructed by incorporating modified silica gel into a conventional graphite paste electrode. The functional group attached to the (3-chloropropyl) silica gel surface was 2-mercaptoimidazole, giving a new product denoted by 3-(2-thioimidazolyl)propyl silica gel, which is able to complex mercury ions. Mercury was chemically adsorbed on the modified graphite paste electrode containing 3-(2-thioimidazolyl)propyl silica (TIPSG GPE) by immersion in a Hg(II) solution, and the resultant surface was characterized by cyclic and differential pulse anodic stripping voltammetry. One cathodic peak at 0.1 V and other anodic peak at 0.34 V were observed on scanning the potential from -0.1 to 0.8 V (0.01 M KNO3; ν = 2.0 mV s-1 νs. Ag/AgCl). The anodic peak at 0.34 V show an excellent sensitivity for Hg(II) ions in the presence of several foreign ions. A calibration graph covering the concentration range from 0.02 to 2 mg L-1 was obtained. The detection limit was estimated to be 5 μg L-1. The precision for six determinations of 0.05 and 0.26 mg L-1 Hg(II) was 3.0 and 2.5% (relative standard deviation), respectively. The method can be used to determine the concentration of mercury(II) in natural waters contaminated by this metal. 2005 © The Japan Society for Analytical Chemistry.
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The aim of this study was to analyze, under scanning electron microscopy (SEM), the morphologic characteristics of root surfaces after application of CarisolvTM gel in association with scaling and root planing (SRP). Sixty periodontally compromised extracted human teeth were randomly assigned to 6 groups: 1) SRP alone; 2) passive topical application of CarisolvTM + SRP; 3) active topical application of CarisolvTM + SRP; 4) multiple applications of CarisolvTM + SRP; 5) SRP + 24% EDTA; 6) topical application of CarisolvTM + SRP + 24% EDTA. CarisolvTM gel was applied to root surfaces for 30 s, followed by scaling and root planing, consisting of 50 strokes with Gracey curettes in an apical-coronal direction, parallel to the long axis of the tooth. The only exception was group 4, in which the roots were instrumented until a smooth, hard and glass-like surface was achieved. All specimens were further analyzed by SEM. The results showed that the treatment with CarisolvTM caused significant changes in root surface morphology of periodontally compromised teeth only when the chemical agent was actively applied (burnishing technique). CarisolvTM failed to remove the smear layer completely, especially with a single application, independently of the method of application. Multiple applications of CarisolvTM were necessary to achieve a smear layer reduction comparable to that obtained with 24% EDTA conditioning.
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This work presents a method to obtain B-scan images based on linear array scanning and 2R-SAFT. Using this technique some advantages are obtained: the ultrasonic system is very simple; it avoids the grating lobes formation, characteristic in conventional SAFT; and subaperture size and focussing lens (to compensate emission-reception) can be adapted dynamically to every image point. The proposed method has been experimentally tested in the inspection of CFRP samples. © 2010 American Institute of Physics.
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Modified fluorcanasite glasses were fabricated by either altering the molar ratios of Na 2O and CaO or by adding P 2O 5 to the parent stoichiometric glass compositions. Glasses were converted to glass-ceramics by a controlled two-stage heat treatment process. Rods (2 mm x 4 mm) were produced using the conventional lost-wax casting technique. Osteoconductive 45S5 bioglass was used as a reference material. Biocompatibility and osteoconductivity were investigated by implantation into healing defects (2 mm) in the midshaft of rabbit femora. Tissue response was investigated using conventional histology and scanning electron microscopy. Histological and histomorphometric evaluation of specimens after 12 weeks implantation showed significantly more bone contact with the surface of 45S5 bioglass implants when compared with other test materials. When the bone contact for each material was compared between experimental time points, the Glass-Ceramic 2 (CaO rich) group showed significant difference (p = 0.027) at 4 weeks, but no direct contact at 12 weeks. Histology and backscattered electron photomicrographs showed that modified fluorcanasite glass-ceramic implants had greater osteoconductivity than the parent stoichiometric composition. Of the new materials, fluorcanasite glass-ceramic implants modified by the addition of P 2O 5 showed the greatest stimulation of new mineralized bone tissue formation adjacent to the implants after 4 and 12 weeks implantation. © 2010 Wiley Periodicals, Inc.
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A new device for irrigation, which presents hydrodynamic activation based on the pressure-suction technology, has recently been introduced to the market: the Rinsendo system. This study compared the efficacy of the Rinsendo system and conventional (manualdynamic) irrigation in the removal of debris from the root canal walls, using scanning electron microscopy (SEM). Twenty mandibular premolars with completely formed roots were selected and randomly divided into group 1 (irrigation with the Rinsendo system) and group 2 (conventional irrigation). The canals were irrigated with 1 ml of saline at each change of instrument. instrumentation started with a #15 K file and continued up to a #40 K file, which was standardized as the working length instrument. Then, the teeth were sectioned in buccolingual direction and the halves were sputter-coated with gold and examined by SEM. The apical, middle and cervical root canal thirds were evaluated, and the results were analyzed statistically by the Mann-Whitney test for comparison between methods, Kruskal-Wallis test for comparison among thirds, and Miller test for individual comparisons. A significance level of 5% was set for all analyses. The results did not show significant differences (p>0.05) between methods at each third and among thirds for each technique analyzed individually. in conclusion, there was no difference in the cleaning ability of the Rinsendo system and conventional irrigation.
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Voltammetric analysis of amodiaquine using a hemin biosensor revealed a well-defined peak at 0.14 V (vs. Ag/AgCl), corresponding to the oxidation of amodiaquine at pH 7.0. The electrodic behavior indicated that the oxidation process was irreversible, and that it was controlled by diffusion. In addition to advantages such as high selectivity and sensitivity, the method developed could be used for the analysis of breast milk containing amodiaquine without any need for prior sample treatment, an important consideration in routine analysis laboratories. Measurements of the drug contained in breast milk were used to validate the technique. The detection limit for standard solutions was 3.30 mg L-1, and the quantification limit was 11.0 mg L-1. ©The Electrochemical Society.
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A major UK initiative, entitled 'Mapping the Underworld', is seeking to address the serious social, environmental and economic consequences arising from an inability to locate the buried utility service infrastructure without resorting to extensive excavations. Mapping the Underworld aims to develop and prove the efficacy of a multi-sensor device for accurate remote buried utility service detection, location and, where possible, identification. One of the technologies to be incorporated in the device is low-frequency vibro-acoustics, and the application of this technology for detecting buried infrastructure is currently being investigated. Here, a shear wave ground vibration technique for detecting buried pipes is described. For this technique, shear waves are generated at the ground surface, and the resulting ground surface vibrations measured, using geophones, along a line traversing the anticipated run of the pipe. Measurements were made at a test site with a single pressurized polyethylene mains water pipe. Time-extended signals were employed to generate the illuminating wave. Cross-correlation functions between the measured ground velocities and a reference measurement adjacent to the excitation were then calculated and summed using a stacking method to generate a cross-sectional image of the ground. The wide cross-correlation peaks caused by high ground attenuation were partially compensated for by using a generalized cross-correlation function called the smoothed coherence transform. To mitigate the effects of other potential sources of vibration in the vicinity, the excitation signal was used as an additional reference when calculating the generalized cross-correlation functions. For two out of three tests, the pipe was detected, indicating that this technique will be a valuable addition to the Mapping the Underworld armoury.
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A voltammetric method for the determination of ethyl acetate in ethanol fuel using a Fe3+/Nafion®-coated glassy carbon electrode (GCE) is proposed. The ethyl acetate present in the ethanol fuel was previously converted to acetohydroxamic acid via pretreatment with hydroxylamine chloride. The acetohydroxamic acid promptly reacted with the iron (III) present in the film, producing iron (III) acetohydroxamate, which presents a well-defined voltammetric peak current at -0.02 V. Optimization of the voltammetric parameters for the cyclic, linear sweep, square wave, and differential pulse modalities was carried out for this chemically-modified electrode. Square wave voltammetry afforded the best response for acetohydroxamic acid detection. The analytical curve for this species was linear from 9 to 100 μmol L 1 according to the following equation: ip (μA) = 0.27 + 2.55Cacetohydroxamic acid (μmol L 1), with linear correlation coefficient equal to 0.993. The technique presented limit of detection equal to 5.3 μmol L 1 and quantification limit of 17.6 μmol L 1. The proposed method was compared to the official method of ethyl acetate analysis (Gas Chromatography), and a satisfactory correlation was found between these techniques. © 2012 Elsevier Ltd. All rights reserved.
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Correlative fractography is a new expression proposed here to describe a new method for the association between scanning electron microscopy (SEM) and light microscopy (LM) for the qualitative and quantitative analysis of fracture surfaces. This article presents a new method involving the fusion of one elevation map obtained by extended depth from focus reconstruction from LM with exactly the same area by SEM and associated techniques, as X-ray mapping. The true topographic information is perfectly associated to local fracture mechanisms with this new technique, presented here as an alternative to stereo-pair reconstruction for the investigation of fractured components. The great advantage of this technique resides in the possibility of combining any imaging methods associated with LM and SEM for the same observed field from fracture surface. © Microscopy Society of America 2013.
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Objective To describe the technique of deep anterior lamellar keratoplasty (DALK) with Descemet's membrane (DM) exposure in horse eyes. Also, to compare the efficacy and safety of viscodissection and big-bubble techniques for DALK. Animals studied Thirty-four ex vivo horse eyes. Procedure Deep anterior lamellar keratoplasty was performed in 34 ex vivo horse eyes. Two groups (Group V - viscodissection - 2% sodium hyaluronate; Group A - air - big-bubble) of 17 eyes were studied. Other than the substance used, the surgical technique was similar for both groups. Nonperforated eyes were submitted for light microscopic histologic evaluation and scanning electron microscopic (SEM) analysis. Results Group V - Perforations occurred in 18% of the eyes during surgery. Light microscopy revealed exposure of DM in 28% of the eyes with mean thickness of the remaining stroma being 70.4μm. Group A - Perforations occurred in 42% of the eyes. Light microscopy revealed exposure of DM in 60% of the eyes with mean thickness of the remaining stroma being 23.3μm. No significant differences in safety, efficacy and thickness of the remaining stroma (including all eyes or excluding those with DM exposure) were observed. SEM of the surgical site revealed a more even surface in those eyes with DM exposure compared to eyes with thicker remaining stroma in both groups. Conclusions We describe two DALK techniques (viscodissection and big-bubble) for use in horses. No significant differences in safety, efficacy and thickness of the remaining stroma were observed. However, a nonsignificant trend toward the big-bubble technique being more efficacious but less safe was observed. © 2012 American College of Veterinary Ophthalmologists.
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The aim of this study was to evaluate the effect of final irrigation protocols (17% EDTA, BioPure MTAD, SmearClear, and QMiX) on microhardness and erosion of root canal dentin. Fifty roots were sectioned transversely at the cement-enamel junction and each root was sectioned horizontally into 4-mm-thick slices. The samples were divided into five groups (n=10) according to the final irrigation protocol: G1: distilled water (control group); G2: 17% EDTA; G3: BioPure MTAD; G4: SmearClear; and G5: QMiX. The dentin microhardness was then measured with a load of 25 g for 10 s. Initially, the reference microhardness values were obtained for the samples without any etching. The same samples were then submitted to the final irrigation protocols. A new measure was realized and the difference between before and after the procedures was the dentin microhardness reduction. In sequence, the specimens were submitted to SEM analysis to verify the dentinal erosion. The Kruskal Wallis and Dunn tests (α=5%) were used to compare the results. The dentin microhardness decreased for all final irrigation protocols. There was no significant difference between groups 2, 3, 4, and 5 (P>0.05), but this groups presented significant dentin microhardness reduction than G1 (P<0.05). In G2, occurred the highest incidence of dentinal erosion (P<0.05). 17% EDTA, BioPure MTAD, SmearClear, and QMiX promoted significant dentin microhardness reduction. © 2013 Wiley Periodicals, Inc.