Simultaneous voltammetric determination of paracetamol and caffeine in pharmaceutical formulations using a boron-doped diamond electrode

A simple and highly selective electrochemical method was developed for the single or simultaneous determination of paracetamol (N-acetyl-p-aminophenol, acetaminophen) and caffeine (3,7-dihydro-1,3,7-trimethyl-1H-purine-2,6-dione) in aqueous media (acetate buffer, pH 4.5) on a boron-doped diamond (BDD) electrode using square wave voltammetry (SWV) or differential Pulse voltammetry (DPV). Using DPV with the cathodically pre-treated BDD electrode, a separation of about 550 mV between the peak oxidation potentials Of paracetamol and caffeine present in binary mixtures was obtained. The calibration curves for the simultaneous determination of paracetamol and caffeine showed an excellent linear response, ranging from 5.0 x 10(-7) mol L(-1) to 8.3 x 10(-7) mol L(-1) for both compounds. The detection limits for the simultaneous determination of paracetamol and caffeine were 4.9 x 10(-7) mol L-1 and 3.5 x 10(-8) mol L(-1), respectively. The proposed method Was Successfully applied in the simultaneous determination of paracetamol and caffeine in several pharmaceutical formulations (tablets), with results similar to those obtained using a high-performance liquid chromatography method (at 95% confidence level). (C) 2008 Elsevier BY. All rights reserved.

Estudo do calor específico de compostos Heusler paramagnéticos, da série do níquel Ni 2 Tal, onde T=Ti, Zr, Hf, V, Nb e Ta

Neste trabalho apresentamos os resultados experimentais da medida do calor específico dos compostos Heusler da série Ni2TA1, onde T =Ti, Zr,Hf,V,Nb, Ta. Estas medidas foram feitas utilizando-se um calorímetro adiabático que atua na faixa de 1,84 K a 10,3 K e visaram o estudo da estrutura elêtrônica dos compostos em termos da densidade de estados eletrônicos à nível de Fermi, bem como da dinâmica da rede cristalina, com o uso dos modelos de Debye e de Einstein para o calor específico. Apresentamos, também, uma descrição do calorímetro, seu funcionamento e as alterações ocorridas em função deste trabalho.

Caracterização por microscopia eletrônica do aço SAE1141 microligado ao Nb

Este trabalho visa a investigação dos aspectos microestruturais, de cunho significativo nas propriedades mecânicas de um aço microligado, através da utilização de técnicas de microscopia eletrônica. Variações em parâmetros de produção e processamento de aços microligados produzem efeitos microestruturais diversos, os quais influenciam diretamente nas propriedades do material. Para tanto, é de suma importância a realização de um acompanhamento da evolução microestrutural de forjados, para que se possa entender os mecanismos de reforço estrutural, e assim, buscar controlá-los. Foram simuladas as condições industriais de forjamento em amostras de aço microligado ao nióbio, SAE 1141, utilizando um simulador termomecânico Gleeble. Esse aço é empregado na produção de garfos (terminal) forjados pela indústria automobilística. As variáveis controladas na simulação foram a temperatura de pré-aquecimento, percentual de deformação e taxa de resfriamento. Os aspectos microestruturais resultantes foram analisados por microscopia de luz visível e eletrônica de varredura. Especial atenção foi dada ao estudo dos aspectos subestruturais através da técnica de microscopia eletrônica de transmissão. Foram utilizadas para tal amostras do tipo réplica de extração em filme de carbono e lâminas finas Os estudos realizados neste trabalho poderão contribuir para otimização do processo de forjamento nessa classe de aços visando garantir boas propriedades mecânicas. Análises por nano-sonda EDS indicam a presença de partículas ricas em Nb. Foi constatado que a temperatura de pré-aquecimento para forjamento desempenha papel importante, pois a temperatura mais baixa, verifica-se fina precipitação de carbonitretos e o refino de grão é mais pronunciado. Este efeito é influenciado também pelo grau de deformação a quente.

Synthesis and characterization of lanthanum- and yttrium-doped Fe2O3 pigments

MELO, D. M. A. et al. Synthesis and charactezarion of lanthanum and yttrium doped Fe2O3 pigments. Cerâmica, São Paulo, v. 53, p. 79-82, 2007.

Caracterização de compósitos Nb-20%cu obtidos por moagem de alta energia e sinterizados por fase líquida

In this work, was studied the formation of a composite of the refractory metal niobium with copper, through the process of high-energy milling and liquid phase sintering. The HEM can be used to synthesize composite powders with high homogeneity and fine size particle distribution. It may also produce the solid solubility in immiscible systems such as Nb-Cu, or extend the solubility of systems with limited solubility. Therefore, in the immiscible system Cu-Nb, the high-energy milling was successfully used to obtain the composite powder particles. Initially, the formation of composite particles during the HEM and the effect of preparation technique on the microstructure of the material was evaluated. Four loads of Nb and Cu powders containing 20%wt Cu were synthesized by MAE in a planetary type ball mill under different periods of grinding. The influence of grinding time on the metal particles is evaluated during the process by the withdrawal of samples at intermediate times of milling. After compaction under different forces, the samples were sintered in a vacuum furnace. The liquid phase sintering of these samples prepared by HEM produced a homogeneous and fine grained. The composite particles forming the sintered samples are the addition of a hard phase (Nb) with a high melting point, and a ductile phase (Cu) with low melting point and high thermal and electrical conductivities. Based on these properties, the Nb-Cu system is a potential material for many applications, such as electrical contacts, welding electrodes, coils for generating high magnetic fields, heat sinks and microwave absorbers, which are coupled to electronic devices. The characterization techniques used in this study, were laser granulometry, used to evaluate the homogeneity and particle size, and the X-ray diffraction, in the phase identification and to analyze the crystalline structure of the powders during milling. The morphology and dispersion of the phases in the composite powder particles, as well the microstructures of the sintered samples, were observed by scanning electron microscopy (SEM). Subsequently, the sintered samples are evaluated for density and densification. And finally, they were characterized by techniques of measuring the electrical conductivity and microhardness, whose properties are analyzed as a function of the parameters for obtaining the composite

Estudo sobre a redução aluminotérmica de Ta2O5 e TiO2 usando descarga de cátodo oco

In this study it was used two metallic oxides, Ta2O5 and TiO2, in order to obtain metallic powders of Ta and Ti through aluminothermic reduction ignited by plasma. Ta2O5 and TiO2 powders were mixed with Al in a planetary mill, using different milling times. A thermal analysis study (DTA and TG) was carried out, in order to know the temperature to react both the mixtures. Then, these mixtures were submitted to a hollow cathode discharge, where they were reacted using aluminothermic reduction ignited by plasma. The product obtained was characterized by XRD and SEM, where it was proven the possibility of producing these metallic particles, different from the conventional process, where metallic ingots are obtained. It was verified that the aluminothermic reduction ignited by plasma is able to produce metallic powders of Ta and Ti, and a higher efficiency was observed to the process with Ta2O5-Al mixtures. Among different microstructural aspects observed, it can be noted the presence of metallic nanoparticles trapped into an Al2O3 matrix, besides acicular structures (titanium) and dendritic structures (tantalum), which are a product characteristic from a fast cooling

Síntese hidrotérmica assistida por micro-ondas de tiO2, e aplicação em nanocompósito

In recent decades have seen a sharp growth in the study area of nanoscience and nanotechnology and is included in this area, the study of nanocomposites with self-cleaning properties. Since titanium dioxide (TiO2) has high photocatalytic activity and also antimicrobial, self-cleaning surfaces in your application has been explored. In this study a comparison was made between two synthesis routes to obtain TiO2 nanoparticles by hydrothermal method assisted by microwave. And after analysis of XRD and SEM was considered the best material for use in nanocomposites. It was deposited nanocomposite film of poly (dimethyl siloxane) (PDMS) with 0.5, 1, 1.5 and 2% by weight of nanoparticles of titanium dioxide (TiO2) by the spraying method. The nanocomposite was diluted with hexane and the suspension was deposited onto glass substrate, followed by curing in an oven with forced air circulation. The photocatalytic activity of the nanocomposite impregnated with methylene blue was evaluated by UV- vis spectroscopy from the intensity variation of absorption main peak at 660nm with time of exposure to the UV chamber. Changes in the contact angle and microhardness were analyzed before and after UV aging test. The effect of ultraviolet radiation on the chemical structure of the PDMS matrix was evaluated by spectrophotometry Fourier transform infrared (FTIR).The results indicated that the addition of TiO2 nanoparticles in the coating PDMS gave high photocatalytic activity in the decomposition of methylene blue, an important characteristic for the development of self-cleaning coatings

Ecotoxicology of Nano-TiO2 An Evaluation of its Toxicity to Organisms of Aquatic Ecosystems

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Obtenção de pós de Nb a partir da redução aluminotérmica com ignição por plasma

The aluminothermic reduction consists in an exothermic reaction between a metallic oxide and aluminum to produce the metal and the scum. The extracted melted metal of that reaction usually comes mixed with particles of Al2O3 resulting of the reduction, needing of subsequent refine to eliminate the residual impure as well as to eliminate porosities. Seeking to obtain a product in powder form with nanometric size or even submicrometric, the conventional heat source of the reaction aluminothermic , where a resistor is used (ignitor) as ignition source was substituted, for the plasma, that acts more efficient way in each particle of the sample. In that work it was used as metallic oxide the niobium pentoxide (Nb2O5) for the exothermal reaction Nb2O5 + Al. Amounts stoichiometric, substoichiometric and superestoichiometric of aluminum were used. The Nb2O5 powder was mixed with aluminum powder and milled in planetarium of high energy for a period of 6 hours. Those powders were immerged in plasm that acts in a punctual way in each particle, transfering heat, so that the reaction can be initiate and spread integrally for the whole volume of the particle. The mixture of Nb2O5 + Al was characterized through the particle size analysis by laser and X-ray diffraction (DRX) and the obtained product of reaction was characterized using the electronic microscopy of sweeping (MEV) and the formed phases were analyzed by DRX. Niobium powders with inferior sizes to 1 mm were obtained by that method. It is noticed, through the analysis of the obtained results, that is possible to accomplish the aluminothermic reduction process by plasma ignition with final particles with inferior sizes to the original oxide

Redução carbotérmica de TiO2 por descarga em cátodo oco

In this study we used the plasma as a source of energy in the process of carbothermic reduction of rutile ore (TiO2). The rutile and graphite powders were milled for 15 h and placed in a hollow cathode discharge produced by in order to obtain titanium carbonitride directly from the reaction, was verified the influence of processing parameters of plasma temperature and time in the synthesis of TiCN. The reaction was carried out at 600, 700 and 800˚C for 3 to 4 hours in an atmosphere of nitrogen and argon. During all reactions was monitored by plasma technique of optical emission spectroscopy (EEO) to check the active species present in the process of carbothermal reduction of TiO2. The powder obtained after the reactions were characterized by the techniques of X-ray diffraction (XRD) and scanning electron microscopy (SEM). The technique of EEO were detected in all reactions the spectra CO and NO, and these gas-phase resulting from the reduction of TiO2. The results of X-ray diffraction confirmed the reduction, where for all conditions studied there was evidence of early reduction of TiO2 through the emergence of intermediate oxides. In the samples reduced at 600 and 700˚C, there was only the phase Ti6O11, those reduced to 800˚C appeared Ti5O9 phases, and Ti6O11 Ti7O13, confirming that the carbothermal reduction in plasma, a reduction of the ore rutile (TiO2) in a series of intermediate titanium oxide (TinO2n-1) where n varies between 5 and 10

Layer by layer TiO2 thin films and photodegradation of Congo red

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Synthesis and structural characterization of Eu(III)-doped Zn7Sb2O12

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

Study of the potentiometric response of the doped spinel Li1.05Al0.02Mn1.98O4 for the optimization of a selective lithium ion sensor

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Development of an electrochemical sensor for potassium ions based on KSr(2)Nb(5)O(15) modified electrode

In the work described by this paper, we studied the development of a selective potassium ion sensor constituted of a carbon paste electrode modified (CPEM) with a novel KSr(2)Nb(2)O(15). The material KSr(2)Nb(2)O(15) is an oxide with the tetragonal tungsten bronze structure (TTB) type are in forefront both in the area of research as well as in industrial applications. The sensor response to potassium ions was linear in the concentration range 1.26 x 10(-5) at 1.62 x 10(-3) mol L(-1) (E (mV) = 32.7 + 51.1 log [K(+)]). The sensor based KSr(2)Nb(2)O(15), of the TTB-type presented very good potentiometric response, with a slope of 51.1 mV/dec (at 25 degrees C) and detection limit for the potassium ions of 7.27 x 10(-5) mol.L(-1)

Influence of the Substitutional Solute on the Mechanical Properties of Ti-Nb Binary Alloys for Biomedical Use

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)