Determination of cadmium in river water samples by flame AAS after on-line preconcentration in mini-column packed with 2-aminothiazole-modified silica gel

A rapid and sensitive method was developed to determine trace levels of Cd2+ ions in an aqueous medium by flame atomic absorption spectrometry, using on-line preconcentration in a mini-column packed with 100 mg of 2-aminothiazol modified silica gel (SiAT). The Cd2+ ions were sorbed at pH 5.0. The preconcentrated Cd2+ ions were directly eluted from the column to the spectrometer's nebulizer-burner system using 100 μL of 2 mol L-1 hydrochloric acid. A retention efficiency of over 95% was achieved. The enrichment factor (calculated as the ratio of slopes of the calibration graphs) obtained with preconcentrations in a mini-column packed with SiAT (A = -1.3 × 10-3 + 1.8 × 10-3 [Cd2+]) and without preconcentrations (A = 4 × 10-5 + 3.5 × 10-3[Cd2+]), was 51 and the detection limit calculated was 0.38 μg L-1. The preconcentration procedure was applied to determine trace levels of Cd in river water samples. The optimum preconcentration conditions are discussed herein.

Preconcentration and determination of mercury(II) at a chemically modified electrode containing 3-(2-thioimidazolyl)propyl silica gel

A mercury-sensitive chemically modified graphite paste electrode was constructed by incorporating modified silica gel into a conventional graphite paste electrode. The functional group attached to the (3-chloropropyl) silica gel surface was 2-mercaptoimidazole, giving a new product denoted by 3-(2-thioimidazolyl)propyl silica gel, which is able to complex mercury ions. Mercury was chemically adsorbed on the modified graphite paste electrode containing 3-(2-thioimidazolyl)propyl silica (TIPSG GPE) by immersion in a Hg(II) solution, and the resultant surface was characterized by cyclic and differential pulse anodic stripping voltammetry. One cathodic peak at 0.1 V and other anodic peak at 0.34 V were observed on scanning the potential from -0.1 to 0.8 V (0.01 M KNO3; ν = 2.0 mV s-1 νs. Ag/AgCl). The anodic peak at 0.34 V show an excellent sensitivity for Hg(II) ions in the presence of several foreign ions. A calibration graph covering the concentration range from 0.02 to 2 mg L-1 was obtained. The detection limit was estimated to be 5 μg L-1. The precision for six determinations of 0.05 and 0.26 mg L-1 Hg(II) was 3.0 and 2.5% (relative standard deviation), respectively. The method can be used to determine the concentration of mercury(II) in natural waters contaminated by this metal. 2005 © The Japan Society for Analytical Chemistry.

Synthesis and characterization of 0.9PMN-0.1PT powders by the use of a modified columbite precursor

The complex perovskite compound 0.9PbMg 1/3Nb 2/3O 3-0.1PbTiO 3 is one of the most promising relaxor ceramic because the addition of lead titanate increases T m, by about 5°C/mol% from intrinsic T m value for pure PMN (near -7 to -15°C). A Ti-modified columbite precursor was used to prepare PMN-PT powders containing single perovskite phase. This variation on columbite route includes Ti insertion in MgNb 2O 6 orthorhombic structure so that individual PT synthesis becomes unnecessary. Furthermore, effects of Li additive on columbite and PMN-PT structures were studied by XRD to verify the phase formation at each processing step. XRD data were also used for the structural refinement by Rietveld method. The additive acts increasing columbite powders crystallinity, and the amount of perovskite phase was insignificantly decreased by lithium addition. By SEM micrographs it was observed that Li presence in PMN-PT powders leads to the formation of rounded primary particles and for lmol% of additive, the grain size is not changed, different from when this concentration is enhanced to 2mol%.

Enhanced photocatalytic reduction of Hg(II) in aqueous medium by 2-aminothiazole-modified TiO2 particles

This work describes the synthesis and characterization of 2-aminothiazole-modified titania and its application on Hg (II) photoreduction in aqueous medium. Infrared spectroscopy confirmed the chemical modification of the titania matrix. The number of 2-aminothiazole groups attached to the titania was determined by Kjeldahl's method. The photocatalytic experiments were carried out in a cylindrical photoreactor thermostatted at 298 K. The resulting modified photocatalyst 2-aminothiazole titania (TiAT) revealed an enhance in the Hg (II) photoreduction capacity at studied pH values (3, 7 and 9). In addition, sorption studies showed that the photocatalyst TiAT presented a lower equilibrium time and a higher sorption capacity of Hg(II) ion, demonstrating that sorption plays a fundamental role in the photoreduction mechanism. ©2006 Sociedade Brasileira de Química.

Preparation of lanthanum doped Bi4Ti3O12 ceramics by the polymeric precursor method

Lanthanum-modified bismuth titanate, Bi4 - xLaxTi3O12 (BLT) ceramics, with x ranging from 0 to 0.75 were prepared by the polymeric precursor method. Orthorhombicity of the system is decreased with the increase of lanthanum content in the bismuth titanate (BIT) crystal lattice. No secondary phases were evident after lanthanum addition. Increasing lanthanum content causes a structural distortion in the bismuth titanate lattice. The shape of the grains is strongly influenced by the lanthanum added to the system. © 2005 Elsevier B.V. All rights reserved.

Screen-printed carbon electrode modified with poly-L-histidine applied to voltammetric determination of chromium (VI)

The present work reports the use of a screen-printed carbon electrode (SPCE) modified by poly-L-histidine film to determine chromium (VI). Stable films can be formed by direct addition of PH solution 1 % (w/v) on the electrode surface, followed by heating at 80°C during 5 min. Calibration curves can be constructed for Cr(VI) from 1.0 × 10-5 mol L-1 to 7.0 × 10-5 mol L-1 Cr (VI) in acetate buffer pH 4 using a preconcentration step of 60s at open circuit potential. A relative standard deviation of 3.2% was for five determination of 4.0 × 10 -5 mol L-1 Cr (VI). The method was successful applied to determination of Cr(VI) in wastewater samples from a leather dyeing industry. copyright The Electrochemical Society.

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.

How the delphi and AHP methods are aiding to define the critical success factors priorities in a digital factory project implementation

Digital factory is a concept that offers a collaborative approach to enhance product and production engineering processes through simulation. Products, processes and resources are modeled to be used to develop and test the product conception and manufacturing processes, before their use in the real factory. The purpose of this paper is to present the steps to identify the Critical Success Factors (CSF) priorities in a digital factory project implementation in a Brazilian company and how the Delphi and AHP Methods are aiding to identify these CSF priorities. Copyright © 2008 SAE International.

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.

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.