SiO2/TiO2 nanostructured composites with three different ratios of Si:Ti were prepared using the sol-gel method. These materials were characterized using energy dispersive X-ray fluorescence, Fourier transform infrared spectroscopy, X-ray diffraction, scanning electron microscopy, high-resolution transmission electron microscopy, photoluminescence, Raman with Fourier transform infrared spectroscopy, and the specific surface area. The band gaps of materials were determined by diffuse reflectance spectra, and the values of 3.20 ± 0.01, 2.92 ± 0.02, and 2.85 ± 0.01 eV were obtained as a result of the proportional increases in the amount of Ti within the composite. The materials exhibit only the anatase (TiO2) crystalline phase and have crystalline domains ranging from 4 to 5 nm. The photodegradation process of methylene blue, royal blue GRL, and golden yellow GL dyes were studied with respect to their contact times, pH variations within the solution, and the variations in the dye concentration of the solution in response to only sunlight. The maximum amount of time for the mineralization of dyes was 90 min. The kinetics of the process follows an apparently first order model, in which the obtained rate constant values were 5.72 × 10-2 min-1 for methylene blue, 6.44 × 10-2min-1 for royal blue GRL, and 1.07 × 10-1min-1 for golden yellow.

Um eletrodo íon seletivo foi construído e avaliado para determinação de íons amônio em águas naturais. O eletrodo consiste de uma pasta de carbono com o compósito SiO2/ZrO2/fosfato-NH4+ obtido pelo processo de sol-gel. O eletrodo exibe uma resposta sub-Nenstiana para concentrações entre 7,7<FONT FACE=Symbol>´</FONT>10-7 e 4,0<FONT FACE=Symbol>´</FONT>10-2 mol L-1 e um limite de detecção de 1,58<FONT FACE=Symbol>´</FONT>10-7 mol L-1 (8,5<FONT FACE=Symbol>´</FONT>10-3 ppm). A resposta do eletrodo foi rápida (1 minuto). Os coeficientes de seletividade KpotA,B para os diversos íons geralmente presentes em águas naturais foram determinados pela aplicação do matched potential method. O método potenciométrico com o eletrodo íon seletivo foi validado pelo método de Berthelot (método padrão) pela determinação de íons amônio em águas naturais. O eletrodo íon seletivo provou ser satisfatório para o controle de qualidade de águas naturais.

Ion selective-electrode was constructed and evaluated for determination of ammonium ions in natural waters. The electrode consists of paste carbon with the composite SiO2/ZrO2/phosphate-NH4+ obtained through sol-gel process. The electrode exhibits a sub-Nernstian response for ammonium concentrations between 7.7<FONT FACE=Symbol>´</FONT>10-7 and 4.0<FONT FACE=Symbol>´</FONT>10-2 mol L-1 and a detection limit of 1.58<FONT FACE=Symbol>´</FONT>10-7 mol L-1 (8.5<FONT FACE=Symbol>´</FONT>10-3 ppm). The electrode response for ammonium was fast (1 minute). The selectivity coefficients KpotA,B for several ions usually present in natural waters were determined applying the matched potential method. The potentiometric method with the ion selective electrode was validated by the Berthelot method (standard method), through the determination of ammonium ions in natural waters. The ion selective-electrode proved suitable for routine quality control of natural waters by potentiometry.

Um novo polímero, cloreto de 3-n-propilpiridínio-silsesquioxano (SiPy+Cl-), foi utilizado na preparação de um eletrodo. Este eletrodo íon seletivo, formado de um bastão de grafite recoberto pelo polímero, foi construído e avaliado pela determinação de Cr(VI) em amostras de águas residuárias de indústrias de galvanoplastia e de couro. O eletrodo exibiu uma resposta Nernstiana para Cr(VI) entre as concentrações 3,1<FONT FACE=Symbol>´</FONT>10-6 e 1,8<FONT FACE=Symbol>´</FONT>10-2 mol L-1 e limite de detecção de 2,8<FONT FACE=Symbol>´</FONT>10-6 mol L-1 (0,15 ppm). A resposta do eletrodo para Cr(VI) foi rápida (15 s) e o potencial independente do pH na faixa de 3,0 a 7,0. Os coeficientes de seletividade para diversos ânions mostram que o eletrodo apresenta um excelente desempenho. O sensor exibe um tempo de vida útil de 6 meses com boa reprodutibilidade. A determinação de Cr(VI) em águas residuárias de indústrias de galvanoplastia e de couro usando o sensor foi realizada com sucesso.

A new polymer, silsesquioxane 3-n-propylpyridinium chloride (SiPy+Cl-), was used in the preparation of an electrode. The polymer coated graphite rod ion selective electrode for Cr(VI) was constructed and evaluated for the determination of Cr(VI) in samples of electroplating and leather industry wastes. This electrode exhibited a Nernstian response for Cr(VI) concentrations between 3.1<FONT FACE=Symbol>´</FONT>10-6 and 1.8<FONT FACE=Symbol>´</FONT>10-2 mol L-1 and a detection limit of 2.8<FONT FACE=Symbol>´</FONT>10-6 mol L-1 (0.15 ppm). The response of the electrode for Cr(VI) was fast (15 s) and the independent potential of pH in the range of 3.0 to 7.0. The selectivity coefficients for several anions showed that the electrode presents excellent performance. The sensor exhibits a shelf-life of 6 months with good reproducibility. Determination of Cr(VI) in electroplating and leather wastes using the sensor was successfully achieved.

The use of sol-gel materials to develop new biosensors has received great attention due to its characteristics and versatility of sol-gel process. An overview is presented of the state-of-the-art of electrochemical biosensors employing sol-gel materials. Low-temperature, porous sol-gel ceramics represent a new class for the immobilization of biomolecules. The rational design of sol-gel sensing materials, based on the judicious choice of the starting alkoxide, encapsulated reagents, and preparation conditions, allows tailoring of material properties in a wide range, and offers great potential for the development of electrochemical biosensors.

Uma superfície de grafite bem polida foi recoberta com um filme fino do polímero cloreto de n-propilpiridínio silsesquioxano. Sobre o filme do polímero fortemente aderido ao grafite, a espécie eletroativa [Fe(CN)6]4- foi adsorvida por meio de uma reação de troca iônica. O eletrodo resultante, (graph/SiPy+)4[Fe(CN)6 ]4- (graph = grafite e SiPy+ representa o polímero N-propilpiridinio silsesquioxano), mostrou-se quimicamente muito estável e foi utilizado para oxidar eletrocataliticamente o ácido ascórbico em solução de KCl 0,1 mol dm-3, em pH entre 4,5 e 6,5. O eletrodo foi utilizado para determinar vitamina C em tabletes e em sucos de laranja processados. Os resultados mostraram uma boa concordância com aqueles obtidos utilizando o método padrão de titulação com 2,6-diclorofenolindofenol.

A well polished graphite surface was coated with a thin film of N-propylpyridinium chloride silsesquioxane polymer. On to the strongly graphite-adhered polymer film the electroactive species [Fe(CN)6]4- was adsorbed by means of an ion exchange reaction. The resulting electrode (graph/SiPy+)4[Fe(CN)6 ]4- (graph = graphite and SiPy+ represents the N-propilpyridinium silsesquioxane polymer) was chemically very stable and was used to electrocatalytically oxidize ascorbic acid in solution (pH between 4.5-6.5) in 0.1 mol dm-3 KCl. The electrode was used to determine vitamin C in tablets and in processed orange juices. The results were in accord with those obtained by using the standard 2,6-dichlorophenolindophenol titration method.