Desenvolvimento de biossensores enzimáticos amperométricos para a determinação de compostos de importância clínica

Este trabalho descreve a preparação e caracterização de eletrodos modificados com azul da Prússia e materiais relacionados e a sua aplicação na construção de biossensores enzimáticos amperométricos para a detecção de oxalato e de glicose. Os materiais utilizados na modificação dos eletrodos foram azul da Prússia e compostos híbridos formados por hexacianoferrato de níquel e polipirrol ou hexacianoferrato de cobre e polipirrol. Os materiais lubridos mostraram-se capazes de mediar na eletroredução de peróxido de hidrogênio, mesmo em eletrólitos contendo Na+, apresentando melhor desempenho analítico quando comparados aos respectivos hexacianoferratos sem a presença do polímero condutor. Estes materiais foram utilizados com êxito na construção de biossensores para oxalato e para glicose, imobilizando as enzimas Oxalato Oxidase e Glicose Oxidase, respectivamente. Também foi estudada a preparação de um biossensor para a detecção de glicose utilizando a técnica de automontagem eletrostática camada por camada. Esta técnica permite otimizar o processo de immobilização da enzima, obtendo excelente desempenho analítico com pouca quantidade de enzima. Finalmente, são apresentadas a síntese, caracterização e aplicação de nanopartículas de azul da Prússia na determinação de peróxido de hidrogênio. Foi possível preparar nanopartículas com um diâmetro médio de 5 nm, as quais foram imobilizadas em eletrodos mediante a técnica de automontagem eletrostática camada por camada, a fim de estudar seu comportamento eletroquímico.

Molecular mixed-valence cyanide bridged Co-III-Fe-II complexes

Cyano-bridged mixed-valence compounds have been known for a long time, i.e., Prussian Blue polymeric solids. Nevertheless, the interest in discrete complexes having a well-defined molecular nuclearity has emerged more recently. There are numerous examples of cyano-bridged mixed-valence complexes in the recent literature, as they show promising and useful applications in electrochromism, molecular magnetism and molecular electronics. In this paper, the reactivity, synthetic and structural chemistry, as well as some physical and chemical properties, of a series of discrete dinuclear mixed-valence cyano-bridged complexes of general formulae [LnCoIII(mu NC)Fe-II(CN)(5)](-) (L = pentadentate macrocyclic ligand) are reviewed. Special emphasis is given to the synthetic strategy, redox properties and metal-to-metal-charge-transfer (MMCT) band energy. Tuning the MMCT transition energy has been possible by changing the redox potential of the metal centers, both through structural and outer-sphere changes. The redox processes that involve the appearance and disappearance of these MMCT bands in the visible region have been dealt with in relation to the possible uses of the complexes. (c) 2004 Elsevier B.V. All rights reserved.

Avaliação das condições de precipitação do azul da Prússia sobre pó de grafite visando o desenvolvimento de eletrodos de pasta de carbono para a quantificação de nitrito

An amperometric FIA method for nitrite quantification based on nitrite electroreduction and employing a carbon paste electrode (CPE) chemically modified with iron hexacyanoferrate (HCF) as an amperometric detector was developed. The influence of experimental conditions on the preparation of the electrode materials was evaluated and the materials obtained in each study were used for the development of modified electrodes. The electrochemical sensors were prepared by a fast, simple, and inexpensive procedure, and the long-term performance of the electrodes were quite satisfactory as the stability was maintained over one year. HCF was an effective redox mediator for nitrite electroreduction in acidic media, allowing nitrite detection at +0.2 V vs. Ag/AgClsat, which is a potential free of possible interfering species that are normally present in food and water samples. The electrochemical cell used in the FIA system was similar to a batch injection analysis cell, enabling recirculation of the carrier solution. This is an attractive feature because it allows the use of a high flow rate (6 mL min-1) leading to high sensitivity and analysis speed, while keeping reagent consumption low. The proposed method had a detection limit of 9 μmol L-1 and was successfully employed for nitrite quantification in spiked water and sausage samples. The obtained results were in good agreement with those provided by the spectrophotometric official method. At a 95 % confidence level it was not observed statistical differences neither in nitrite content nor in the precision provided by both methods. The experimental conditions for the synthesis of HCF were optimized and the best electrode material was prepared by mixing FeCl3, K4[Fe(CN)6] and carbon powder subjected to an acid and thermal treatment (400 ºC), followed by ultrasonic agitation at 4 °C. This material was used to construct an electrode with improved analytical performance to reduce nitrite, which presented greater stability compared to HCF film electrodeposited on the EPC, showing that the preparation procedure of the electrode material is an effective strategy for the development of HCF modified electrodes.

Aluminum and iron can be deposited in the calcified matrix of bone exostoses.

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Synthesis and characterization of low-cost materials for aqueous Na-ion batteries

136 p.

SbOx thin films used for write-once blue laser recording

SbOx thin films are deposited by reactive dc-magnetron sputtering from all antimony metal target in Ar+O-2 with the relative O-2 content 7%. It is found that the as-deposited films call represent a two-component system comprising amorphous Sb and amorphous Sb2O3. The crystallization of Sb is responsible for the changes of optical properties of the films. The results of the static, test show that the SbOx thin films have good writing sensitivity for blue laser beams and the recording marks are very clear and circular. High reflectivity contrast of about 41% is obtained at a writing power 6 mW and writing pulse width 300 ns. In addition, the films show a good stability after reading 10000 times.

Write-once blue laser recording using silicon doped SbOx thin films prepared by reactive dc-magnetron sputtering

Si:SbOx films have been deposited by reactive dc-magnetron sputtering from a Sb target with Si chips attached in Ar + O-2 with the relative O-2 content 7%. The as-deposited films contained Sb metal, Sb2O3, SiO, Si2O3 and SiO2. The crystallization of Sb was responsible for the changes of optical properties of the films. The results of the blue laser recording test showed that the films had good writing sensitivity for blue laser beam (406.7 nm), and the recording marks were still clear even if the films were deposited in air 60 days, which demonstrated that doping silicon in SbOx films can improve the stability of SbOx films. High reflectivity contrast of about 36% was obtained at a writing power 6 mW and writing pulse width 300 ns. (c) 2007 Elsevier B.V. All rights reserved.

Write-once medium with Fe-Doped BiOx thin films for blue laser recording

Fe:BiOx films are fabricated on K9 glass substrates by rf-magnetron sputtering of a BiFeO target under argon atmosphere with increasing sputtering power from 80 to 200 W at room temperature. It is found that the thin films grown at the sputtering power of 160W can be formed at an appropriate deposition rate and have an improved surface morphology. The XPS result reveals that the films investigated are comprised of Bi, Fe and O elements. A typical XRD pattern shows that no phase transition occurs in the films up to 400 degrees C. The results of the blue laser recording test demonstrate that the Fe:BiOx films have good writing sensitivity for blue laser beam (406.7 nm) and good stability after reading 10000 times. The recording marks of 200nm or less are obtained. These results indicate that the introduction of Fe into BiOx films can reduce the mark size and improve the stability of the films.

Role of edge dislocation and Si impurity in linking the blue luminescence and yellow luminescence in n-type GaN films

A close relationship is found between the blue and yellow luminescence bands in n-type GaN films, which are grown without intentional acceptor doping. The intensity ratio of blue luminescence to yellow luminescence (I-BL/I-YL) decreases with the increase in edge dislocation densities as demonstrated by the (102) full width at half maximum of x-ray diffraction. In addition, the I-BL/I-YL ratio decreases with the increase in Si doping. It is suggested that the edge dislocation and Si impurity play important roles in linking the blue and yellow luminescence.

Violet/blue emission from hydrogenated amorphous carbon films deposited from energetic CH3+ ions and ion bombardment

Considering the complexity of the general plasma techniques, pure single CH3+ ion beams were selected for the deposition of hydrogenated amorphous (a) carbon films with various ion energies and temperatures. Photoluminescence (PL) measurements have been performed on the films and violet/blue emission has been observed. The violet/blue emission is attributed to the small size distribution of sp(2) clusters and is related to the intrinsic properties of CH3 terminals, which lead to a very high barrier for the photoexcited electrons. Ion bombardment plays an important role in the PL behavior. This would provide further insight into the growth dynamics of a-C:H films. (C) 2002 American Institute of Physics.

Blue-violet luminescence double peak of In-doped films prepared by radio frequency sputtering

ZnO films doped with different contents of indium were prepared by radio frequency sputtering technique. The structural, optical and emission properties of the films were characterized at room temperature using XRD, XPS, UV-vis-NIR and PL techniques. Results showed that the indium was successfully incorporated into the c-axis preferred orientated ZnO films, and the In-doped ZnO films are of over 80% optical transparency in the visible range. Furthermore, a double peak of blue-violet emission with a constant energy interval (similar to 0.17 eV) was observed in the PL spectra of the samples with area ratio of indium chips to the Zn target larger than 2.0%. The blue peak comes from the electron transition from the Zn-i level to the top of the valence band and the violet peak from the In-Zn donor level to the V-Zn level, respectively.

Realization of blue, green and red emission from top-emitting white organic light-emitting diodes with exterior tunable optical films

We developed an approach to realize blue, green and red emission from top-emitting white organic light-emitting diodes (OLEDs) through depositing exterior tunable optical films on top of the OLEDs. Three primary colors for full color display including blue, green and red emission are achieved by controlling the wavelength-dependent transmittance of the multilayer optical films overlaid on the emissive layer.

Simultaneous blue, green, and red emission from diblock copolymer micellar films: a new approach to white-light emission

White-light emission is achieved from a single layer of diblock copolymer micelles containing green- and red-light-emitting dyes in the separate micellar cores and blue-light-emitting polymer around their periphery, in which fluorescence resonance energy transfer between fluorophores is inhibited due to micelle isolation, resulting in simultaneous emission of these three species.