Resumo em Inglês:

The complexes of 4-chlorophenoxyacetates of Mn(II), Co(II), Ni(II) and Cu(II) have been synthesized as polycrystalline solids, and characterized by elemental analysis, spectroscopy, magnetic studies and also by X-ray diffraction and thermogravimetric measurements. The analysed complexes have the following colours: pink for Co(II), green for Ni(II), blue for Cu(II) and a pale pink for Mn(II) compounds. The carboxylate group binds as monodentate and bidentate ligands. On heating to 1173K in air the complexes decompose in several steps. At first, they dehydrate in one step to anhydrous salts, that next decompose to the oxides of respective metals. Their magnetic moments were determined in the range of 76-303K. The results reveal them to be high-spin complexes of weak ligand fields.

Resumo em Inglês:

MgO is an important inorganic material, which can be used in many aspects, such as catalyst, toxic-waste remediation agent, adsorbent, and others. In order to make use of MgO, nano-MgO was prepared by ultrasonic method using Mg (CH3COO)2.2H2O as precursor, NaOH aqueous solution as precipitant in this paper. Effect factors on MgO nano-particle size were investigated. Characteristics of samples were measured by TGA, XRD, TEM, and others techniques. The results showed that the size of nano-MgO about 4 nm could be obtained under the following conditions (ultrasonic time 20 min, ultrasonic power 250 W, titration rate of NaOH 0.25 mL/min, NaOH concentration 0.48 mol/L, calcinations temperature 410 °C, calcination time 1.5 h, heating rate of calcination 5 °C/min). It was a very simple and effective method to prepare nano-MgO.

Resumo em Inglês:

Semiempirical calculations at the level of PM3 of theory were carried out to study the structural and electronic properties of C80 and some of its doped derivatives with the elements of group III and V at the level of PM3 of theory. We have selected these elements to be substituted in the fullerene-C80 cage in order to show the effect of such structural change on the electronic properties of the molecules studied. The theoretical IR spectra, some of physical and chemical properties of the molecules studied are obtained and discussed.

Resumo em Inglês:

Stability constant (log beta) and thermodynamic parameters of Cd2+ complexes with sulfonamide and cephapirin were determined by Polarographic technique at pH = 7.30 ± 0.01 and µ = 1.0 M KNO3 at 250°C. The sulfonamides were sulfadiazine, sulfisoxazole, sulfamethaxazole, sulfamethazine, sulfathiazole, sulfacetamide and sulfanilamide used as primary ligands and cephapirin as secondary ligand. Cd2+ formed 1:1:1, 1:2:1 and 1:1:2 complexes. The nature of electrode processes were reversible and diffusion controlled. The stability constants and thermodynamic parameters (deltaG, deltaH and deltaS) were determined. The formation of the metal complexes has been found to be spontaneous, exothermic in nature, and entropically unfavourable at higher temperature.

Resumo em Português:

No presente trabalho os parâmetros de desempenho (validação intralaboratorial) da metodologia de determinação de TPH (Total Petroleum Hydrocarbons) foram determinados por detecção na região do infravermelho com o equipamento da Infracal TOG/TPH, visando aplicação em amostras de areia contaminadas com petróleo. Os ensaios foram realizados utilizando Óleo Marine Fuel 380, com densidade igual 0,987 g cm-3 e viscosidade de 5313 cP a 20°C. Este óleo foi fornecido pelo Centro de Pesquisa da Petrobrás (CENPES/PETROBRÁS/RJ), sendo o mesmo óleo derramado no acidente ocorrido em janeiro de 2000, na Baia de Guanabara, RJ, quando 1.300 m3 vazaram do duto que interliga a REDUC (Refinaria Duque de Caxias, RJ) ao terminal da Ilha d’Água/RJ, atingindo praias. Os resultados da validação indicaram que o desempenho da metodologia foi favorável à aplicação que se destina. Entre os parâmetros metrológicos obtidos neste trabalho, o limite de detecção do método foi de 4,06 mg L-1, consideravelmente inferior à faixa de concentração normalmente obtida para amostras em tais situações.

Resumo em Inglês:

This work deals with an optimization of TPH (Total Petroleum Hydrocarbon) analysis methodology for samples of contaminated sands, validating the infrared detection technique through the use of Infracal TOG/TPH equipment. Tests were validated using Marine Fuel 380 oil, density 0.987 g cm-3 and viscosity 5313 cP at 20 ºC. This oil sample was kindly supplied by Petrobras Research Centre (CENPES), and is the same oil that leaked from a pipeline in REDUC Refinery on January 2000, contaminating several beaches in Guanabara Bay, including Anil and Mauá. The validation results suggested that the methodology performance was adequate for this application. Amongst the metrological parameters obtained from this work, the detection limit, 4.06 mg L-1, was a plus; since it was far below to the concentration range obtained from this samples.

Resumo em Português:

Foram sintetizados no estado sólido os compostos Ln-Bz, onde Ln representa lantanídeos trivalentes e Bz benzoato. Análise termogravimétrica e análise térmica diferencial (TG/DTA) foi usada para estudar a decomposição térmica destes compostos em atmosfera de CO2.

Resumo em Inglês:

Solid-state Ln-Bz compounds, where Ln stands for trivalent lanthanides and Bz is benzoate have been synthesized. Simultaneous thermogravimetric and differential thermal analysis in a CO2 atmosphere were used to study the thermal decomposition of these compounds.

Resumo em Português:

De acordo com a Resolução nº 54 da Agência Nacional de Vigilância Sanitária (ANVISA), os limites máximos permitidos para níquel e chumbo em água mineral natural e água natural são 20 µg L-1 e 10 µg L-1, respectivamente. O presente trabalho apresenta o potencial de uso da técnica de espectrometria de absorção atômica em chama com fonte contínua e de alta resolução (HR-CS FAAS) na determinação seqüencial rápida de níquel e chumbo para fins de análise classificatória de água mineral de acordo com a ANVISA. Duas linhas de absorção atômica foram empregadas para níquel (232,003 nm - principal e 341,477 nm - secundária) e chumbo (217,0005 nm - principal e 283,306 nm - secundária) e diferentes volumes de linha (número de pixels). Em geral, a sensibilidade melhorou com o aumento do número de pixels e com a soma das absorbâncias das linhas atômicas estudadas. As principais figuras de mérito obtidas com a técnica HR-CS FAAS foram comparadas com a espectrometria de absorção atômica em chama com fonte de linhas (LS FAAS). As amostras de água mineral foram evaporadas antes de serem analisadas de modo a obter um fator de pré-concentração de aproximadamente cinco vezes. As recuperações de Pb variaram significativamente com o aumento do volume das linhas. As melhores recuperações foram observadas na linha principal (92-93%) e na somatória de ambas (90-92%). No caso do Ni, esta influência foi pouco relevante, sendo que a recuperação variou de 92-104%.

Resumo em Inglês:

National Health Surveillance Agency (ANVISA) established in the decree number 54 maximum allowed levels for Ni and Pb in mineral and natural waters at 20 µg L-1 and 10 µg L-1, respectively. For screening analysis purposes, the high-resolution continuum source flame atomic absorption spectrometry technique (HR-CS FAAS) was evaluated for the fast-sequential determination of nickel and lead in mineral waters.Two atomic lines for Ni (232.003 nm - main and 341.477 nm - secondary) and Pb (217.0005 nm - main and 283.306 nm - secondary) at different wavelength integrated absorbance (number of pixels) were evaluated. Sensitivity enhanced with the increase of the number of pixels and with the summation of the atomic lines absorbances. The main figures of merit associated to the HR-CS FAAS technique were compared with that obtained by line-source flame atomic absorption spectrometry (LS FAAS). Water samples were pre-concentrated about 5-fold by evaporation before analysis. Recoveries of Pb significantly varied with increased wavelength integrated absorbance. Better recoveries (92-93%) were observed for higher number of pixels at the main line or summating the atomic lines (90-92%). This influence was irrelevant for Ni, and recoveries in the 92-104% range were obtained in all situations.

Resumo em Português:

O comportamento eletroquímico da enzima peroxidase (HRP) foi estudado utilizando o peróxido de hidrogênio como substrato enzimático e o ácido 5-aminossalicílico (5-ASA) como mediador de elétrons sobre eletrodo de grafite. Diversos parâmetros foram otimizados, tais como, o potencial aplicado à técnica amperométrica fixado em -0,125V, a solução tampão fosfato-citrato 0,1 mol L-1 pH 5,0 como eletrólito suporte e a proporção entre o 5-ASA e H2O2 em 1:7, entre outros. Foi observada a catálise da reação de oxidação do peróxido de hidrogênio na presença da enzima HRP e do mediador 5-ASA. O produto dessa oxidação foi reduzido na superfície do eletrodo, evidenciando um significativo aumento na intensidade da corrente catódica.

Resumo em Inglês:

The electrochemical behavior of the enzyme peroxidase (HRP) was investigated using the hydrogen peroxide as enzymatic substrate and the 5-aminosalicylic acid (5-ASA) as mediator of electrons on graphite electrodes. Several parameters were optimized, namely, the applied potential to the amperometric technique fixed in -0.125V, the 0.1 mol L-1 phosphate-citrate buffer at pH 5.0 as supporting electrolyte and the proportion between the 5-ASA and H2O2 in 1:7, among others. It was observed the catalysis of the oxidation reaction of the H2O2 in the presence of the enzyme HRP and 5-ASA. The oxidation product was reduced in the electrode surface, evidencing a significant increase in the intensity of the cathodic current.

Resumo em Português:

A reação de precipitação de prata na liga Cu-8%Al-6%Ag foi estudada usando medidas de variação da microdureza com a temperatura e o tempo de envelhecimento, difratometria de raios X (DRX), calorimetria exploratória diferencial (DSC), microscopia eletrônica de varredura (MEV). Os resultados obtidos indicaram que o mecanismo da reação de precipitação da prata é um processo controlado pela difusão da prata e a velocidade desta reação atinge um máximo em torno de 500°C.

Resumo em Inglês:

Ag precipitation reaction in the Cu-8wt.%Al-6wt.%Ag alloys was studied using microhardness measurements with temperature and ageing time, X-ray diffraction patterns (DRX), differential scanning calorimetry (DSC) and scanning electron microscopy (SEM). The results obtained showed that the mechanism of Ag precipitation reaction is an Ag diffusion controlled process and reaction rate reaches a maximum at about 500ºC.

Resumo em Inglês:

The structural and electronic properties of 1-(5-Hydroxymethyl - 4 -[ 5 - (5-oxo-5-piperidin- 1 -yl-penta- 1,3 -dienyl)-benzo [1,3] dioxol- 2 -yl]-tetrahydro -furan-2 -yl)-5-methy l-1Hpyrimidine-2,4dione (AHE) molecule have been investigated theoretically by performing density functional theory (DFT), and semi empirical molecular orbital calculations. The geometry of the molecule is optimized at the level of Austin Model 1 (AM1), and the electronic properties and relative energies of the molecules have been calculated by density functional theory in the ground state. The resultant dipole moment of the AHE molecule is about 2.6 and 2.3 Debyes by AM1 and DFT methods respectively, This property of AHE makes it an active molecule with its environment, that is AHE molecule may interacts with its environment strongly in solution.