879 resultados para Electrochemical impedance spectroscopy measurements
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A sensor was fashioned to monitor the volume of nutrient in a solid substrate-based growth media by using electrochemical admittance spectroscopy. Several experimental parameters were investigated (i.e. The use of two- or three-electrode cells, the superficial area of the electrode, the amount of nutrient solution added to the growth media, and the influence of varying the dc and ac potential) to assess how these variables affect the admittance of the system. A linear correlation was observed between the maximum of the imaginary admittance and the volume of nutrient present. The response factor was 2.8 x 10(-5) S cm(-2) ml(-1) and the limit of detection (LOD) was 0.54 ml. The humidity of the growth media does not change the response of the nutrient toward the monitoring measurements. These results demonstrate that the volume of nutrient in this solid substrate-based growth media can be assessed using a ceramic sensor to measure the imaginary admittance. (C) 2002 Elsevier B.V. B.V. All rights reserved.
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The electrochemical behavior of the annealed Cu-5wt.%Ni alloy in 0.5 M H2SO4 was studied by means of open-circuit potential (E-OCP) measurements, cyclic voltammetry, electrochemical impedance spectroscopy (EIS), and quasi-stationary linear potential sweep. The hydrodynamics of the system was also studied. This material is constituted by a single a, phase. The anodic behavior of a Cu-Ni alloy in H2SO4 consists fundamentally on the electrodissolution of Cu, its main component, and the formation of a sulfur-containing passive layer. The presence of Ni decreases the rate of Cu oxidation, mostly at high positive potentials. The impedance spectra, obtained for the unrotating electrode, can be interpreted in terms of a simple charge-transfer reaction across a surface layer. When the electrode is rotated, the occurrence of an inductive loop evidenced the existence of an adsorbed layer. All the resistance estimated from the proposed equivalent circuits diminished with the electrode rotation rate, emphasizing the influence of ion transport in the overall electrode process. The system presented two anodic Tafel slopes: 40 mV dec(-1) for E < 255 mV and 67 mV dec(-1) for E > 275 mV. A Tafel slope of 40 mV dec(-1) evidences that copper dissolution can be interpreted in terms of the mechanism proposed by Mattsson and Bockris. The second Tafel suggests that at potentials more positive than 275 mV, copper dissolves according to a mechanism that considers the disproportionation of adsorbed Cu(1) species. (C) 2003 Elsevier Ltd. All rights reserved.
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The electrochemical behavior of Cu-xAl alloys, with 11 wt%less than or equal to x less than or equal to 15wt%, in 0.5 M H2SO4 was studied by means of open-circuit potential decay measurements, quasi-stationary and fast cyclic voltammetry, and electrochemical impedance spectroscopy. Some of the alloys (x less than or equal to 14%), when quenched formed martensitic structures. Alloys with greater than or equal to 13% showed a little square-shaped phase when quenched from temperatures around 800 degrees C. It was observed that in sulfuric medium, these formations were dealuminized differently than the martensitic phase. The values of the rest potentials are more influenced by the heat treatment rather than by the alloy composition. An anodic Tafel slope of ca. 60 mV/decade was observed for all the alloys, independently of the heat treatment. This is explained in terms of a competition between two processes: copper oxidation and copper(I) deproportionation. In the cyclic voltammetric experiments it was observed an anodic current peak, related with copper oxidation with a possible formation of some interfacial species, and a cathodic current peak during the reverse potential scan, associated with the reduction of soluble species and/or of the film. The AC Impedance data were interpreted in terms of electric equivalent circuits.
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The electrochemical behavior of a coating of cobalt oxide on cold-rolled steel in alkaline sodium sulfate was Studied using the electrochemical techniques of open-circuit potential measurements and electrochemical impedance spectroscopy. The coating was prepared at different annealing temperatures ranging from 350 to 750 degreesC and characterized by SEM, EDX and XRD. Below 550 degreesC the composition of the coating was basically of Co3O4. At 750 degreesC CoO was formed and big cracks appeared on the film exposing an inner layer of iron oxides. Analysis of the EIS data is very difficult because of the complexity of the interface structure. It can be inferred that the charge transfer resistance of the coatings prepared at 350 and 450 C were higher than those for the coatings prepared at temperatures above 550 degreesC. (C) 2002 Published by Elsevier B.V. Ltd.
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The main goal of the present study was to evaluate the effect of different setting accelerator agents on the developed microstructures of calcium phosphate cements (CPCs) by employing the impedance spectroscopy (IS) technique. Six compositions of CPCs were prepared from mixtures of commercial dicalcium phosphate anhydrous (DCPA) and synthesized tetracalcium phosphate (TTCP) as the solid phases. Two TTCP/DCPA molar ratios (1/1 and 1/2) and three liquid phases (aqueous solutions of Na(2)HPO(4), tartaric acid (TA) and oxalic acid (OA), 5% volume fraction) were employed. Initial (I) and final (F) setting times of the cement pastes were determined with Gillmore needles (ASTM standard C266-99). The hardened samples were characterized by X-ray powder diffraction (XRD), Fourier transformed infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and apparent density measurements. The IS technique was employed as a non-destructive tool to obtain information related to porosity, tortuosity and homogeneity of the cement microstructures. The formulation prepared from a TTCP/DCPA equimolar mixture and OA as the liquid phase presented the shortest I and F (12 and 20 min, respectively) in comparison to the other studied systems. XRD analyses revealed the formation of low-crystallinity hydroxyapatite (HA) (as the main phase) as well as the presence of little amounts of unreacted DCPA and TTCP after 24 h hardening in 100% relative humidity. This was related to the proposed mechanisms of dissolution of the reactants. The bands observed by FTIR allowed identifying the presence of calcium tartrate and calcium oxalate in the samples prepared from TA and OA, in addition to the characteristic bands of HA. High degree of entanglement of the formed crystals was observed by SEM in samples containing OA. SEM images were also correlated to the apparent densities of the hardened cements. Changes in porosity, tortuosity and microstructural homogeneity were determined in all samples, from IS results, when the TTCP/DCPA ratio was changed from 1/1 to 1/2. The cement formulated from an equimolar mixture of TTCP/DCPA and OA as the liquid phase presented setting times, degree of conversion to low-crystallinity HA and microstructural features suitable to be used as potential bone cement in clinical applications. The IS technique was shown to be a very sensitive and non-destructive tool to relate the paste composition to the developed microstructures. This approach could be very useful to develop calcium phosphate bone cements for specific clinical demands.
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)
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The electrochemical behaviour of Cu, Cu-Al and Cu-Al-Ag alloys in aqueous solutions of NaCl (0.5 M, pH = 3.00) was studied by means of voltammetric methods and electrochemical impedance spectroscopy. The surfaces were examined by SEM and EDX analysis. Cu-Al-Ag alloy shows a potentiodynamic behaviour similar to that of the pure copper electrode while the Cu-Al alloy presents some minor differences. In the active dissolution region the electrodes suffer pitting corrosion and in the other potential regions there are the formation of a passivant film with composition depending on the potential. The impedance responses of the electrodes are discussed. An electrodissolution mechanism is proposed and the effect of the alloying elements upon the impedance response and polarisation curves is explained. The main effects are due to the production of copper and silver chlorides and aluminium oxides/ hydroxides at the corroding interface. The addition of Al or (Al + Ag) increases the corrosion resistance of pure copper. © 1995.
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The patination of copper is known for its complexity and heterogeneous formation. For a deeper investigation, a locally resolved surface analysis was considered. An exact determination of the accessed area and a potentiostatic control in a three-electrode configuration was reached with the use of the electrochemical microcell technique, which enables local electrochemical measurement such as local electrochemical impedance spectroscopy and cyclic voltammetry. Such a technique provides a unique way for performing the investigation of heterogeneities on electrode surfaces. The local electrochemical measurements on the artificially patinated surface have allowed distinguishing areas of different reactivity even when the analysis of the surface revealed a homogenous chemical composition of patina. Local measurements with the electrochemical microcell showed the presence of small defects on the patina layer that can be modelled by considering a hemispherical diffusion process at small active areas surrounded by larger less reactive domains.
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Die transmembrane Potenzialdifferenz Δφm ist direkt mit der katalytischen Aktivität der Cytochrom c Oxidase (CcO) verknüpft. Die CcO ist das terminale Enzym (Komplex IV) in der Atmungskette der Mitochondrien. Das Enzym katalysiert die Reduktion von O2 zu 2 H2O. Dabei werden Elektronen vom natürlichen Substrat Cytochrom c zur CcO übertragen. Der Eleltronentransfer innerhalb der CcO ist an die Protonentranslokation über die Membran gekoppelt. Folglich bildet sich über der inneren Membrane der Mitochondrien eine Differenz in der Protonenkonzentration. Zusätzlich wird eine Potenzialdifferenz Δφm generiert.rnrnDas Transmembranpotenzial Δφm kann mit Hilfe der Fluoreszenzspektroskopie unter Einsatz eines potenzialemfindlichen Farbstoffs gemessen werden. Um quantitative Aussagen aus solchen Untersuchungen ableiten zu können, müssen zuvor Kalibrierungsmessungen am Membransystem durchgeführt werden.rnrnIn dieser Arbeit werden Kalibrierungsmessungen von Δφm in einer Modellmembrane mit inkorporiertem CcO vorgestellt. Dazu wurde ein biomimetisches Membransystem, die Proteinverankerte Doppelschicht (protein-tethered Bilayer Lipid Membrane, ptBLM), auf einem transparenten, leitfähigem Substrat (Indiumzinnoxid, ITO) entwickelt. ITO ermöglicht den simultanen Einsatz von elektrochemischen und Fluoreszenz- oder optischen wellenleiterspektroskopischen Methoden. Das Δφm in der ptBLM wurde durch extern angelegte, definierte elektrische Spannungen induziert. rnrnEine dünne Hydrogelschicht wurde als "soft cushion" für die ptBLM auf ITO eingesetzt. Das Polymernetzwerk enthält die NTA Funktionsgruppen zur orientierten Immobilisierung der CcO auf der Oberfläche der Hydrogels mit Hilfe der Ni-NTA Technik. Die ptBLM wurde nach der Immobilisierung der CcO mittels in-situ Dialyse gebildet. Elektrochemische Impedanzmessungen zeigten einen hohen elektrischen Widerstand (≈ 1 MΩ) der ptBLM. Optische Wellenleiterspektren (SPR / OWS) zeigten eine erhöhte Anisotropie des Systems nach der Bildung der Doppellipidschicht. Cyklovoltammetriemessungen von reduziertem Cytochrom c bestätigten die Aktivität der CcO in der Hydrogel-gestützten ptBLM. Das Membranpotenzial in der Hydrogel-gestützten ptBLM, induziert durch definierte elektrische Spannungen, wurde mit Hilfe der ratiometrischen Fluoreszenzspektroskopie gemessen. Referenzmessungen mit einer einfach verankerten Dopplellipidschicht (tBLM) lieferten einen Umrechnungsfaktor zwischen dem ratiometrischen Parameter Rn und dem Membranpotenzial (0,05 / 100 mV). Die Nachweisgrenze für das Membranpotenzial in einer Hydrogel-gestützten ptBLM lag bei ≈ 80 mV. Diese Daten dienen als gute Grundlage für künftige Untersuchungen des selbstgenerierten Δφm der CcO in einer ptBLM.
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OBJECTIVES: Many flow-cytometric cell characterization methods require costly markers and colour reagents. We present here a novel device for cell discrimination based on impedance measurement of electrical cell properties in a microfluidic chip, without the need of extensive sample preparation steps and the requirement of labelling dyes. MATERIALS AND METHODS, RESULTS: We demonstrate that in-flow single cell measurements in our microchip allow for discrimination of various cell line types, such as undifferentiated mouse fibroblasts 3T3-L1 and adipocytes on the one hand, or human monocytes and in vitro differentiated dendritic cells and macrophages on the other hand. In addition, viability and apoptosis analyses were carried out successfully for Jurkat cell models. Studies on several species, including bacteria or fungi, demonstrate not only the capability to enumerate these cells, but also show that even other microbiological life cycle phases can be visualized. CONCLUSIONS: These results underline the potential of impedance spectroscopy flow cytometry as a valuable complement to other known cytometers and cell detection systems.
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In this paper, we investigated the effect of hydrogen termination on the electrical properties and impedance spectra of detonation nanodiamond. The impedance spectra revealed that the hydrogen-termination process increases the electrical conductivity by four orders of magnitude at room temperature. An equivalent circuit has been proposed to correlate with the conduction mechanism. Arrhenius plot showed that there were two different activation energy levels located at 0.089 eV and 0.63 eV between 50 °C and 400 °C. The possible physical mechanism corresponding to these activation energy levels has been discussed. Hydrogen-terminated detonation nanodiamond has been further annealed at different temperatures prior to FTIR and XPS measurements in order to understand their thermal stability. The results demonstrated that the surface oxidization occurred between 100 °C and 150 °C. However, the C-H bonds could partially survive when the temperature reaches 400 °C in air. © 2013 American Institute of Physics.