Methodology for DSC calibration in high heating rates

Despite the large use of differential scanning calorimetry (DSC) technique in advanced polymer materials characterization, the new methodology called DSC in high heating rates was developed. The heating rate during conventional DSC experiments varying from 10 to 20°C.min-1, sample mass from 10 to 15mg and standard aluminum sample pan weighting, approximately, 27mg. In order to contribute to a better comprehension of DSC behavior in different heating rates, this work correlates as high heating rate influences to the thermal events in DSC experiments. Samples of metallic standard (In, Pb, Sn and Zn) with masses varying from 0.570mg to 20.9mg were analyzed in multiples sample heating rate from 4 to 324°C. min-1. In order to make properly all those experiments, a precise and careful temperature and enthalpy calibrations were performed and deeply discussed. Thus, this work shows a DSC methodology able to generate good and reliable results on experiments under any researcher choice heating rates to characterize the advanced materials used, for example, for aerospace industry. Also it helps the DSC users to find in their available instruments, already installed, a better and more accurate DSC test results, improving in just one shot the analysis sensitivity and resolution. Polypropylene melting and enthalpy thermal events are also studied using both the conventional DSC method and high heating rate method.

Formation of silver chloride nanocrystals as a corrosion product of silver in H2SO4 solution

The purpose of this study is to characterize the corrosion product on the surface of silver, employing H2SO4 (0.5M) as electrolyte. The electrochemical parameters, Ecor, Icor, V cor and Rp were obtained after analyzing the potentiodynamic polarization curve in which two peaks were observed. The smallest (passive region) is attributed to the Cl- traces from the reference electrode, with micro-cracks. The second peak (in the transpassivation region) corresponds to the polarization curve of silver in H2SO 4 without contaminants. SEM images and EDS analysis reveal images of a surface layer on silver, consisting of structures containing sulfur, oxygen, silver and chloride, as the corrosion product. On this layer silver sulfate crystals were observed, which occurs during the formation of silver chloride nanocrystals with different morphologies, when chloride ions were added to the electrolyte medium. ©The Electrochemical Society.

Hydrogen oxidation on ordered intermetallic phases of platinum and tin - A combined experimental and theoretical study

Hydrogen oxidation on the surfaces of the intermetallic compounds Pt 3Sn, PtSn and PtSn2 has been studied by the rotating disc electrode technique. Pt3Sn and PtSn were found to be good catalysts, about as good as Pt, while PtSn2 was inactive over the investigated range of potentials. Underpotential deposition of hydrogen is observed only on Pt3Sn. These results are explained by theoretical calculations based on a theory developed within our own group, and by density functional theory. © 2012 Elsevier B.V.

Low tungsten content of nanostructured material supported on carbon for the degradation of phenol

A comparative study using different mass proportions of WO3/C (1%, 5%, 10% and 15%) for H2O2 electrogeneration and subsequent phenol degradation was performed. To include the influence of the carbon substrate and the preparation methods, all synthesis parameters were evaluated. The WO3/C materials were prepared by a modified polymeric precursor method (PPM) and the sol-gel method (SGM) on Vulcan XC 72R and Printex L6 carbon supports, verifying the most efficient metal/carbon proportion. The materials were physically characterized by X-ray diffraction (XRD) and by X-ray photoelectron spectroscopy (XPS) techniques. The XRD and the XPS techniques identified just one phase containing WO3 and elevated oxygen concentration on carbon with the presence of WO3. The oxygen reduction reaction (ORR), studied by the rotating ring-disk electrode technique, showed that WO3/C material with the lowest tungsten content (1% WO3/C), supported on Vulcan XC 72R and prepared by SGM, was the most promising electrocatalyst for H2O2 electrogeneration. This material was then analyzed using a gas diffusion electrode (GDE) and 585mgL-1 of H2O2 was produced in acid media. This GDE was employed as a working electrode in an electrochemical cell to promote phenol degradation by an advanced oxidative process. The most efficient method applied was the photo-electro-Fenton; this method allowed for 65% degradation and 11% mineralization of phenol during a 2-h period. Following 12h of exhaustive electrolysis using the photo-electro-Fenton method, the total degradation of phenol was observed after 4h and the mineralization of phenol approached 75% after 12h. © 2013 Elsevier B.V.

Estudos não-isotérmicos da cinética de nucleação e cristalização de vidros 20Li2O80TeO2

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Desenvolvimento e estudo de nanocatalisadores bimetálicos para catodos de células a combustível

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Preparação e teste de nanocatalisadores 'PTFENI'/'C' e 'PTFECO'/'C' para redução de oxigênio

Pós-graduação em Química - IQ

New voltammetry-based analytical method for indirect determination of procymidone in brazilian apples

Procymidone, a potentially carcinogenic and mutagenic pesticide, can contribute to environmental and human contamination when applied to apple crops. In this work, we propose a reliable and sensitive method to determine procymidone in Brazilian apples. The method involves differential pulse (DPV) and square-wave voltammetry (SWV) techniques on a glassy carbon electrode. In a supporting electrolyte solution of 0.5 mol L−1 NaOH, procymidone undergoes an irreversible one-electron oxidation at +1.42 V by cyclic voltammetric vs. Ag|AgCl, KCl 3 M reference electrode. The proposed DPV and SWV methods have a good linear response in the 8.00–20.0 mg L−1 range, with limits of detection (LOD) of 0.678 and 0.228 mg L−1, respectively, in the absence of the matrix. We obtained improved LOD (0.097 mg L−1) in the presence of apple matrix and the supporting electrolyte solution. We used three commercial apple samples to evaluate recovery, and we achieved recovery percentages ranging from 94.6 to 110 % for procymidone determinations. We also tested the proposed voltammetric method for reproducibility, repeatability, and potential interferents, and the results were satisfactory for electroanalytical purposes.

Desenvolvimento de metodologia para determinação de álcoois superiores em álcool combustível, utilizando a técnica de cromatografia líquida de alta eficiência com detecção eletroquímica

Pós-graduação em Química - IQ

Desenvolvimento de método para determinação de acetaldeído em álcool etílico hidratado combustível por cromatografia líquida de alta eficiência com detecção eletroquímica

Pós-graduação em Química - IQ

Concentração de flúor nas refeições e saúde bucal de crianças matriculadas em creches públicas

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Desenvolvimento de métodos analíticos para a determinação da concentração de fosfito em fertilizantes

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Desenvolvimento de métodos eletroanalíticos para determinação de compostos nitrogenados em combustíveis derivados do petróleo

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Estudo de composições vítreas no sistema ternário Ga-Ge-Te para o armazenamento de dados

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Cell membrane integrity of candida albicans after different protocols of microwave irradiation

To evaluate the ability of low time microwaveexposureto inactivate and damage cell membrane integrity of C. albicans. Materials and Methods: Two 200ml C. albicans suspensions were obtained. Sterile dentures were placed in a beaker containing Experimental (ES) or Control suspensions (CS). ES was microwaved at 650 W for 1, 2, 3, 4 or 5 min. Suspensions were optically counted using Methylene blue dye as indicative of membrane-damaged cells; spread on Agar Sabouraud dextrose (ASD) for viability assay; or spectrophotometrically measured at 550nm. Cell-free solutions were submitted to content analyses of protein (Bradford and Pyrogallol red methods); Ca++ (Cresolphthalein Complexone method); DNA (spectrophotometer measurements at 260nm) and K+ (selective electrode technique). Data were analyzed by Student-t test and linear regression (α=0.05). In addition, flowcytometry analysis of Candida cells in suspensionwas performed using propidium iodide. Results: All ES cells demonstrated cell membrane damage at 3, 4 and 5 min,viable cells were nonexistent at 3, 4 and 5 min ES ASD plates and optical density of ES and CS was not significantly differentfor all exposition times. ES cells released highcontents of protein, K+ , Ca++ and DNA after 2 min exposition when compared to that of the CSs. Similar results were observed with flow cytometry analysiswith regard to the periodsof microwave exposure. Conclusions: Microwave irradiation inactivated C. albicansafter 3min and damaged cell membrane integrity after 2 min exposition.