Direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirits by graphite furnace AAS using tungsten permanent modifier with co-injection of Pd/Mg(N03)2

A method was developed using the multi-element graphite furnace atomic absorption spectrometry technique for the direct and simultaneous determination of As, Cu, and Pb in Brazilian sugar cane spirit (cachaça) samples. Also employed was the end-capped transversely heated graphite atomizer (THGA) with platforms pre-treated with W permanent modifier and co-injection of Pd/Mg(N03)2. Pyrolysis and atomization temperature curves were established in a cachaça medium (1+1; v/v) containing 0.2% (v/v) HN03 and spiked with 20 μg L-1 As and Pb and 200 μg L-1Cu. The effect of the concentration of major elements usually present in cachaça matrices (Ca, Mg, Na, and K) and ethanol on the absorbance of As, Cu, and Pb was investigated. Analytical working solutions of As, Cu, and Pb were prepared in 10% (v/v) ethanol plus 5.0 mg L-1 Ca, Mg, Na, and K. Acidified to 0.2% (v/v) HNO3, these solutions were suitable to build calibration curves by matrix matching. The proposed method was applied to the simultaneous determination of As, Cu, and Pb in commercial sugar cane spirits. The characteristic mass for the simultaneous determination was 16 pg As, 119 pg Cu, and 28 pg Pb. The pretreated tube lifetime was about 450 firings. The limit of detection (LOD) was 0.6 μg L-1As, 9.2 μg L-1 Cu, and 0.3 μg L-1Pb. The found concentrations varied from 0.81 to 4.28 μg L-1As, 0.28 to 382 mg L-1 Cu and 0.82 to 518 μg L-1 Pb. The recoveries of the spiked samples varied from 94-112% (As), 97-111% (Cu), and 95-101% (Pb). The relative standard deviation (n=12) was 6.9%, 7.4%, and 7.7% for As, Cu, and Pb, respectively, present in a sample at 0.87 μgL-1, 0.81 mgL-1, and 38.9 μgL-1concentrations.

Bond strength durability of direct and indirect composite systems following surface conditioning for repair

Purpose: This study evaluated the effect of surface conditioning methods and thermocycling on the bond strength between a resin composite and an indirect composite system in order to test the repair bond strength. Materials and Methods: Eighteen blocks (5 x 5 x 4 mm) of indirect resin composite (Sinfony) were fabricated according to the manufacturer's instructions. The specimens were randomly assigned to one of the following two treatment conditions (9 blocks per treatment): (1) 10% hydrofluoric acid (HF) for 90 s (Dentsply) + silanization, (2) silica coating with 30-Ìm SiOx particles (CoJet) + silanization. After surface conditioning, the bonding agent was applied (Adper Single Bond) and light polymerized. The composite resin (W3D Master) was condensed and polymerized incrementally to form a block. Following storage in distilled water at 37°C for 24 h, the indirect composite/resin blocks were sectioned in two axes (x and y) with a diamond disk under coolant irrigation to obtain nontrimmed specimens (sticks) with approximately 0.6 mm2 of bonding area. Twelve specimens were obtained per block (N = 216, n = 108 sticks). The specimens from each repaired block were again randomly divided into 2 groups and tested either after storage in water for 24 h or thermocycling (6000 cycles, 5°C to 55°C). The microtensile bond strength test was performed in a universal testing machine (crosshead speed: 1 mm/min). The mean bond strengths of the specimens of each block were statistically analyzed using two-way ANOVA (α = 0.05). Results: Both surface conditioning (p = 0.0001) and storage conditions (p = 0.0001) had a significant effect on the results. After 24 h water storage, silica coating and silanization (method 2) showed significantly higher bond strength results (46.4 ± 13.8 MPa) than that of hydrofluoric acid etching and silanization (method 1) (35.8 ± 9.7 MPa) (p < 0.001). After thermocycling, no significant difference was found between the mean bond strengths obtained with method 1 (34.1 ± 8.9 MPa) and method 2 (31.9 ± 7.9 MPa) (p > 0.05). Conclusion: Although after 24 h of testing, silica coating and silanization performed significantly better in resin-resin repair bond strength, both HF acid gel and silica coating followed by silanization revealed comparable bond strength results after thermocycling for 6000 times.

Reconfiguration of distribution systems by a modified genetic algorithm

In this paper a genetic algorithm based reconfiguration method is proposed to minimize the real power losses of distribution systems. The main innovation of this research work is that new types of crossover and mutation operators are proposed, such that the best possible results are obtained, with an acceptable computational effort. The crossover and mutation operators were developed so as to take advantage of the particular characteristics of distribution systems (as the radial topology). Simulation results indicate that the proposed method is very efficient, being able to find excellent configurations, with low computational effort, especially for larger systems. ©2007 IEEE.

Optimal power flow via interior-exterior method

This paper presents a new approach to the resolution of the Optimal Power Flow problem. In this approach the inequality constraints are treated by the Modified Barrier and Primal-Dual Logarithmic Barrier methods. The inequality constraints are transformed into equalities by introducing positive auxiliary variables, which are perturbed by the barrier parameter. A Lagrangian function is associated with the modified problem. The first-order necessary conditions are applied to the Lagrangian, generating a nonlinear system which is solved by Newton's method. The perturbation of the auxiliary variables results in an expansion of the feasible set of the original problem, allowing the limits of the inequality constraints to be reached. Numerical tests on the Brazilian CESP and South-Southeast systems and a comparative test indicated that the new approach efficiently resolves of the Optimal Power Flow problem. © 2007 IEEE.

Effect of light-curing method and indirect veneering materials on the Knoop hardness of a resin cement

This study evaluated the Knoop hardness of a dual-cured resin cement (Rely-X ARC) activated solely by chemical reaction (control group) or by chemical / physical mode, light-cured through a 1.5 mm thick ceramic (HeraCeram) or composite (Artglass) disc. Light curing was carried out using conventional halogen light (XL2500) for 40 s (QTH); light emitting diodes (Ultrablue Is) for 40 s (LED); and Xenon plasma arc (Apollo 95E) for 3 s (PAC). Bovine incisors had their buccal face flattened and hybridized. On this surface a rubber mold (5 mm in diameter and 1 mm in height) was bulk filled with the resin cement. A polyester strip was seated for direct light curing or through the discs of veneering materials. After dry storage in the dark (24 h 37°C), the samples (n = 5) were sectioned for hardness (KHN) measurements, taken in a microhardness tester (50 gF load 15 s). The data were statistically analyzed by ANOVA and Tukey's test (α = 0.05). The cement presented higher Knoop hardness values with Artglass for QTH and LED, compared to HeraCeram. The control group and the PAC/Artglass group showed lower hardness values compared to the groups light-cured with QTH and LED. PAC/HeraCeram resulted in the worst combination for cement hardness values. © 2009 Sociedade Brasileira de Pesquisa Odontológica.

Osteoconductivity of modified fluorcanasite glass-ceramics for bone tissue augmentation and repair

Modified fluorcanasite glasses were fabricated by either altering the molar ratios of Na 2O and CaO or by adding P 2O 5 to the parent stoichiometric glass compositions. Glasses were converted to glass-ceramics by a controlled two-stage heat treatment process. Rods (2 mm x 4 mm) were produced using the conventional lost-wax casting technique. Osteoconductive 45S5 bioglass was used as a reference material. Biocompatibility and osteoconductivity were investigated by implantation into healing defects (2 mm) in the midshaft of rabbit femora. Tissue response was investigated using conventional histology and scanning electron microscopy. Histological and histomorphometric evaluation of specimens after 12 weeks implantation showed significantly more bone contact with the surface of 45S5 bioglass implants when compared with other test materials. When the bone contact for each material was compared between experimental time points, the Glass-Ceramic 2 (CaO rich) group showed significant difference (p = 0.027) at 4 weeks, but no direct contact at 12 weeks. Histology and backscattered electron photomicrographs showed that modified fluorcanasite glass-ceramic implants had greater osteoconductivity than the parent stoichiometric composition. Of the new materials, fluorcanasite glass-ceramic implants modified by the addition of P 2O 5 showed the greatest stimulation of new mineralized bone tissue formation adjacent to the implants after 4 and 12 weeks implantation. © 2010 Wiley Periodicals, Inc.

Microscopic and dielectric analyses of vanadium and tungsten modified barium zirconium titanate ceramics

Dielectric spectroscopy was used in this study to examine polycrystalline vanadium and tungstendoped BaZr 0.1Ti 0.90O 3 (BZT10:2V and BZT10:2W) ceramics obtained by the mixed oxide method. According to X-ray diffraction analyses, addition of vanadium and tungsten lead to ceramics free of secondary phases. SEM analyses reveal that both dopants result in slower oxygen ion motion and consequently lower grain growth rate. Temperature dependence dielectric study showed normal ferroelectric to paraelectric transition well above the room temperature for the BZT10 and BZT10:2V ceramics. However, BZT10:2W ceramic showed a relaxor-like behavior near phase transition characterized by the empirical parameter γ. Piezoelectric force microscopy images reveals that the piezoelectric coefficient is strongly influenced by type of donor dopant suggesting promising applications for dynamic random access memories and data-storage media. Copyright © 2010 American Scientific Publishers All rights reserved.

Simple electroanalytical method for determination of guanosine in biological sample

A poly glutamic acid film modified electrode exhibited a catalytic response toguanosine oxidation potential and higher peak current value. Linear concentration curve was obtained in the concentration interval of 1.0 a 10.0 μmol L-1 in 0.04 mol L-1 B-R buffer pH 2.0 with a detection limit of 0.198 μmol L-1. The electrode was used for the determination of guanosine in the potential of +1.1 V (vs. Ag/AgCl) using differential pulse voltammetry (DPV) at urine sample with good recovery. © 2010 by CEE.

Concentration of Cu(II) and Cd(II) from natural river water by Adsorption on a Modified Silica Surface

A high surface area silica gel (737 ± m2 g-1) was synthesized modified through a two-step reaction with a 4-amino-2-mercaptopyrimidine ligand and applied to Cu(II) and Cd(II) adsorption from an aqueous medium. The modified material was characterized by FTIR, which showed that attachment of the molecule occurred via thiol groups at 2547 and 2600 cm-1, and by elemental analysis that indicated the presence of 0.0102 mmol of ligand. The data from adsorption experiments were adjusted to a modified Langmuir equation and the maximum adsorption capacity was 6.6 and 3.8 μmol g-1 for Cu(II) and Cd(II), respectively. After adjusting several parameters, the material was applied in the preconcentration of natural river water using a continuous flow system before and after sample mineralization, and the results showed a 10-fold enrichment factor. The proposed method was validated through preconcentration and analysis of certified standard reference material (1643e), whose results were in agreement with the values provided by the manufacturer.

Numerical correction for the diffuse solar irradiance by the melo-escobedo shadowring measuring method

The present paper deals with numerical corrections factors proposed as a function of the clearness index in order to correct the diffuse solar irradiance measured with the Melo-Escobedo Shadowring Measuring Method (ME shadowring). The global irradiance was measured by an Eppley - PSP pyranometer ; direct normal irradiance by an Eppley-NIP pyrheliometer fitted to a ST-3 sun tracking device and the diffuse irradiance by an Eppley-PSP pyranometer fitted to a ME shadowring. The validations were performed by the MBE and RMSE statistical indicators. The results showed that the numerical correction factors were appropriate to correct the shadowring diffuse irradiance.

PtSnIr/C anode electrocatalysts: Promoting effect in direct ethanol fuel cells

This study investigates the promoting effect of PtSnIr/C (1:1:1) electrocatalyst anode, prepared by polymeric precursor method, on the ethanol oxidation reaction in a direct ethanol fuel cell (DEFC). All of the materials used were 20% metal m/m on carbon. X-ray photoelectron spectroscopy (XPS) analysis showed the presence of Pt, PtOH 2, PtO 2, SnO 2 and IrO 2 at the electrocatalyst surface, indicating a possible decorated particle structure. X-ray diffractometry (XRD) analysis indicated metallic Pt and Ir as well as the formation of an alloy with Sn. Using the PtSnIr/C electrocatalyst prepared here with two times lower loading of Pt than PtSn/C E-tek electrocatalyst, it was possible to obtain the same maximum power density found for the commercial material. The main reaction product was acetic acid probably due to the presence of oxides, in this point the bifunctional mechanism is predominant, but an electronic effect should not be discarded. © 2012 Sociedade Brasileira de Química.

Adapted colorimetric method for measurement of feline urinary glycosaminoglycans

Several methods have been employed to quantify urinary glycosaminoglycans (GAGs), such as chromatography associated with electrophoresis and colorimetric methods, cheaper and faster ones, which employ mainly azure A and B, alcian blue, and dimethylmethylene blue (DMB). The purpose of this study was to standardize a reproducible and cheap method to measure total urinary GAGs in feline urine. Two colorimetric methods based on DMB were tested with chondroitin sulfate C as standard. Urine samples were obtained from 12 healthy cats and some modifications were made for the chosen method to be adequate. The modified technique using DMB acetate buffer carried out in this study can be used to measure feline urinary GAGs. © 2012 Springer-Verlag London.

Electrochemical behavior and voltammetric determination of pyrazinamide using a poly-histidine modified electrode

Pyrazinamide (Pyrazinecarboxamide-PZA) is a drug that is used to treatment tuberculosis. In the present work, the voltammetric behavior of PZA was studied using a screen-printed modified electrode (SPCE). The modified electrode was constructed using poly-histidine films, and it showed an electrocatalytic effect, thus promoting a decrease in PZA reduction potential and improving the voltammetric response. Cyclic voltammetry and electrochemical impedance spectroscopy techniques have been employed in order to elucidate of the electrodic reaction. The results allowed the proposal that in the PZA reduction, a further chemical reaction occurs that corresponds to a second-order process which is subsequent to the electrode reaction. In addition, a sensitive voltammetric method was developed, and it was successfully applied for PZA determination in human urine samples. The best response was found using SPCE modified with poly-histidine prepared by histidine monomer electropolymerization (SPCE/EPH). The electroanalytical performance of the SPCE/EPH was investigated by linear sweep (LSV), differential pulse (DPV), and square wave voltammetry (SWV). A linear relationship between peak current and PZA concentrations was obtained from 9.0 × 10-7 to 1.0 × 10-4 mol L-1 by using DPV. The limit of detection at 5.7 × 10 -7 mol L-1 was estimated, and a relative standard deviation of the 5.0 × 10-6 mol L-1 of PZA of 10 measurement was 3.7%. © 2012 Elsevier B.V. All rights reserved.

Thermal, rheological, and structural behaviors of natural and modified cassava starch granules, with sodium hypochlorite solutions

The use of chemically modified starches is widely accepted in various industries, with several applications. In this research, natural cassava starch granules were treated with standard sodium hypochlorite solution at 0.8, 2.0, and 5.0 g Cl/100 g starch. The native and modified starch samples were investigated by means of the following techniques: simultaneous thermogravimetry-differential thermal analysis, which allowed us to verify the thermal decomposition associated with endothermic or exothermic phenomena; and differential scanning calorimetry that was used to determine gelatinization enthalpy as well as the rapid viscoamylographic analysis that provided the pasting temperature and viscosity. By means of non-contact-atomic force microscopy method and X-ray powder patterns diffractometry, it was possible to observe the surface morphology, topography of starch granules, and alterations in the granules' crystallinity. © 2012 Akadémiai Kiadó, Budapest, Hungary.

Effect of the composition on the thermal behaviour of the SrSn1-xTixO3 precursor prepared by the polymeric precursor method

Strontium stannate titanate Sr(Sn, Ti)O3 is a solid solution between strontium stannate (SrSnO3) and strontium titanate (SrTiO3). In the present study, it was synthesized at low temperature by the polymeric precursor method, derived from the Pechini process. The powders were calcined in oxygen atmosphere in order to eliminate organic matter and to decrease the amount of SrCO3 formed during the synthesis. The powders were annealed at different temperatures to crystallize the samples into perovskites-type structures. All the compositions were studied by thermogravimetry (TG) and differential thermal analysis (DTA), infrared spectroscopy (IR) and X-ray diffraction (XRD). The lattice former, Ti4+ and Sn4+, had a meaningful influence in the mass loss, without changing the profile of the TG curves. On the other hand, DTA curves were strongly modified with the Ti4+:Sn4+ proportion in the system indicating that intermediate compounds may be formed during the synthesis being eliminated at different temperature ranges, while SrCO3 elimination occurs at higher temperature as shown by XRD and IR spectra. © 2013 Akadémiai Kiadó, Budapest, Hungary.