Comparison of the univariate and multivariate methods in the optimization of experimental conditions for determining Cu, Pb, Ni and Cd in biodiesel by GFAAS

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

Adsorption of transition-metal ions in ethanol solution by a nanomaterial based on modified silsesquioxane

The material octakis[3-(3-amino- 1,2,4-triazole)propyl]octasilsesquioxane (ATZ-SSQ) was synthesized and its potential was assessed for Cu(II), Ni(II), Co(II), Zn(II) and Fe(III) from their ethanol solutions and compared with related 3-amino-1,2,4-triazole-propyl modified silica gel (ATZ-SG). The adsorption was performed using a batchwise process and both organofunctionalized surfaces showed the ability to adsorb the metal ions from ethanol solution. The Langmuir model allowed to describe the sorption of the metal ions on ATZ-SSQ and ATTZ-SG in a satisfactory way. The equilibrium is reached very quickly Q min) for ATZ-SSQ, indicating that the adsorption sites are well exposed. The maximum metal ion uptake values for Cu(II), Co(II), Zn(II), Ni(II) and Fe(III) were 0.86, 0.09, 0.19, 0.09 and 0.10 mmol g(-1), respectively, for the ATZ-SSQ, which were higher than the corresponding values 0.21, 0.04, 0.14, 0.05 and 0.07 mmol g(-1) achieved with the ATZ-SG. In order to obtain more information on the metal-ligand interaction of the complexes on the surface of the ATZ-SSQ, Cu(II) was used as a probe to determine the arrangements of the ligands around the central metal ion by electron spin resonance (ESR). The ATZ-SSQ was used for the separation and determination (in flow using a column technique) of the metal ions present in commercial ethanol. (c) 2008 Elsevier B.V. All rights reserved.

Efeitos da suplementação de fitase sobre a disponibilidade aparente de Mg, Ca, Zn, Cu, Mn e Fe em alimentos vegetais para a tilápia-do-nilo

Cem juvenis de tilápia-do-nilo (Oreochromis niloticus; PV = 100.0 ± 5.0 g) foram distribuídos em 10 tanques-rede com o objetivo de avaliar o efeito da suplementação da enzima fitase (0, 1.000 e 2.000 UFA/kg) sobre a disponibilidade de minerais em alguns alimentos energéticos (milho, milho extrusado, farelo de trigo, farelo de arroz e farelo de sorgo) e protéicos (farelo de soja extrusado, farelo de soja, farelo de girassol, farelo de algodão e glúten de milho) utilizados na alimentação de tilápia-do-nilo (Oreochromis niloticus). Para determinação dos coeficientes de disponibilidade aparente (CDA) do cálcio (Ca), magnésio (Mg), zinco (Zn), cobre (Cu), ferro (Fe) e manganês (Mn), foram confeccionadas 31 rações, marcadas com 0,10% de óxido de crômio III uma referência (ração purificada) e 30 contendo os dez alimentos e os diferentes níveis de suplementação da enzima fitase. O CDA dos nutrientes foi calculado com base no teor de crômio da ração e das fezes. A fitase aumenta, nos vegetais, a disponibilidade do Mg, Cu, Zn e Mn, os quais apresentam tendência diferenciada, em razão do seu valor biológico e do nível de suplementação de enzima.

Evaluation of Cu, Mn, and Se in Vegetables Using Ultrasonic Extraction and GFAAS Quantification

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

New analytical procedure based on a cellulose bag and ionic exchanger with p-aminobenzoic acid groups for differentiation of labile and inert metal species in aquatic systems

A new procedure was developed for the in situ characterization of the lability of metal species in aquatic systems by using a system equipped with a diffusion membrane and cellulose organomodified with p-aminobenzoic acid groups (DM-Cell-PAB). To this end, the DM-Cell-PAB system was prepared by adding cellulose organomodified with p-aminobenzoic acid groups (Cell-PAB) to pre-purified cellulose bags. After the DM-Cell-PAB system was sealed, it was examined in the laboratory to evaluate the influence of complexation time, mass of exchanger, pH, metal ions (Cu, Cd, Fe, Mn, and Ni), and concentration of organic matter on the relative lability of metal species. It was found that the pH and kinetics strongly influence the process of metal complexation by the DM-Cell-PAB system. At all pH levels, Cd, Mn, and Ni showed lower complexation with Cell-PAB resin than Cu and Fe metals. Note that relative lability of metals complexed to aquatic humic substances (AHS) in the presence of Cell-PAB resin showed the following order: Cu congruent to Fe >> Ni > Mn=Cd. The results presented here also indicate that increasing the AHS concentration decreases the lability of metal species by shifting the equilibrium to AHS-metal complexes. Our results indicate that the system under study offers an interesting alternative that can be applied to in situ experiments for differentiation of labile and inert metal species in aquatic systems.

Copper determination in ethanol fuel by differential pulse anodic stripping voltammetry at a solid paraffin-based carbon paste electrode modified with 2-aminothiazole organofunctionalized silica

Solid paraffin-based carbon paste electrodes modified with 2-aminothiazole organofunctionalized silica have been applied to the anodic stripping determination of copper ions in ethanol fuel samples without any sample treatment. The proposed method comprised four steps: (1) copper ions preconcentration at open circuit potential directly in the ethanol fuel sample; (2) exchange of the solution and immediate cathodic reduction of the absorbate at controlled potential; (3) differential pulse anodic stripping voltammetry; (4) electrochemical surface regeneration by applying a positive potential in acid media. Factors affecting the preconcentration, reduction and stripping steps were investigated and the optimum conditions were employed to develop the analytical procedure. Using a preconcentration time of 20 min and reduction time of 120 s at -0.3 V versus Ag/AgCl(sat) a linear range from 7.5 x 10(-8) to 2.5 x 10(-6) mol L(-1) with detection limit of 3.1 x 10(-8) mol L(-1) was obtained. Interference studies have shown a decrease in the interference effect according to the sequence: Ni > Zn > Cd > Pb > Fe. However, the interference effects of these ions have not forbidden the application of the proposed method. Recovery values between 98.8 and 102.3% were obtained for synthetic samples spiked with known amounts of Cu(2+) and interfering metallic ions. The developed electrode was successfully applied to the determination of Cu(2+) in commercial ethanol fuel samples. The results were compared to those obtained by flame atomic absorption spectroscopy by using the F-test and t-test. Neither F-value nor t-value have exceeded the critical values at 95% confidence level, confirming that there are no significant differences between the results obtained by both methods. (c) 2006 Elsevier B.V. All rights reserved.

Electrochemical studies of copper-aluminum-silver alloys in 0.5 M H2SO4

The electrochemical behavior in 0.5 M H2SO4 at 25 degreesC of a Cu-Al(9.3 wt%)-Ag(4.7 wt%) alloy submitted to different heat treatments and an annealed Cu- Al(9.7 wt%)-Ag(34.2 wt%) were studied by means of open circuit potential (E-mix) measurements, potentiodynamic polarizations and cyclic voltammetry. SEM and EDX microanalysis were used to examine the changes caused by the electrochemical perturbations. The steady state potentials observed for the studied samples were correlated in terms of the phases present in the alloys surface. The resulting E/I potentiodynamic profiles were explained in terms of the potentiodynamic behavior of pure copper and pure silver. The presence of aluminum decreased the extent of copper oxidation. In the apparent Tafel potential region, two anodic Tafel slopes were obtained: 40 mV dec(-1) in the low potential region and 130 mV dec(-1) in the high potential region, which were related with the electrochemical processes involving copper oxidation. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Aging kinetics in the Cu-8 wt.% Al alloy with Ag additions

The influence of additions of 2, 4, 6, 8, 10 and 12 wt.% Ag in the isothermal aging kinetics of the Cu-8 wt.% Al alloy was studied using microhardness measurements, differential scanning calorimetry, optical and scanning electron microscopy and X-ray diffractometry. The results indicate that the presence of silver is responsible for the shift of the equilibrium concentration to higher Al contents, allowing the formation of the gamma(1) phase (Al4Cu9) in this alloy. For Ag additions up to 6% the dominant kinetic process is Ag precipitation and for additions from 8 to 12% Ag the nucleation of the perlitic phase dominates. (C) 2003 Elsevier B.V. B.V. All rights reserved.

Effect of Ag addition on the martensitic phase of the Cu-10 wt.% Al alloy

Thermal analysis and compression tests at room temperature have been carried out for Cu-10 wt.% Al and Cu-10 wt.% Al-10 wt.% Ag alloys samples. The results indicate that the decomposition reaction of the (beta(1)) parent phase is decreased suppressed and a martensite stabilization effect can be induced by Ag addition. The Cu-Al-Ag alloy shows some degree of shape memory capacity. (C) 2007 Elsevier B.V. All rights reserved.

Kinetics of martensite decomposition in the Cu-9Al-6Ag alloy

The non-occurrence of the beta' -> (alpha+ gamma(1)) decomposition reaction in the Cu-9 wt.% Al-6 wt.% Ag alloy, on ageing between 200 and 450 degrees C, is discussed considering the influence of Ag on point defects redistribution and energy difference between martensite and the ordered parent phase. (c) 2005 Elsevier B.V All rights reserved.

Isothermal decomposition kinetics in the Cu-9%Al-4%Ag alloy

The influence of 4 wt.%Ag addition on the isothermal decomposition kinetics of the beta' phase in the Cu-9wt.%Al alloy was studied by microhardness measurements, optical and scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis, and X-ray diffractometry. The results showed that the presence of Ag decreases the beta' --> (alpha + gamma(1)) decomposition reaction rate in the Cu-9%Al-4%Ag alloy, an effect that may be associated to the gamma(1) phase which catalyses the Ag precipitation, making it faster than the decomposition reaction, and thus, stabilizing the martensitic phase. (C) 2003 Elsevier B.V. All rights reserved.

Thermal stability of the martensitic transformation of Cu-Al-Ni-Mn-Ti

The development of new shape memory alloys with high martensitic transformation temperature increases the potential for applications. The development and use of these new alloys depends on the stability of the structure during cycling at high temperatures. If it is possible to guarantee that on alloys keeps the structure during cycling, then the alloy can be used because of the shape memory properties. The aim of this work is to obtain a kinetic model of the forward and backward martensitic transformation of two Cu-Al-Ni-Mn-Ti alloys. Differential scanning calorimetry has been performed in order to establish the kinetic stability of the martensite and the beta transformation. (c) 2006 Elsevier B.V. All rights reserved.

Isothermal aging kinetics in the Cu-19 at.%Al alloy

The influence of the disordered (Cu)-alpha phase in the isothermal aging kinetics of the Cu-19 at.%Al alloy was studied using microhardness measurements, optical and scanning electron microscopy and X-ray diffractometry. The results indicate that the beta'-->(alpha+gamma (1)) decomposition reaction rate increases with the increase of the temperature in the range between 150 and 500 degreesC and at 600 degreesC the reaction is delayed by the alpha phase precipitation. The value obtained for the activation energy indicates an interface diffusion controlled reaction. (C) 2001 Elsevier B.V. B.V. All rights reserved.

Reverse martensitic transformation in the Cu-10 wt% Al-6 wt%Ag alloy

The reverse martensitic transformation in the Cu-10 wt%Al-6 wt%Ag alloy was studied by classical differential thermal analysis (IDTA), scanning electron microscopy (SEM), energy dispersive X-ray analysis (EDX) and X-ray diffractometry (XRD). The results indicated that the presence of Ag in the Cu-10%Al alloy is responsible for the separation of the competitive reactions that occur during the reverse martensitic transformation and is also associated to an increase in the disordering degree at high temperatures, when compared with alloys without Ag addition. (c) 2005 Springer Science + Business Media, Inc.

A study of the microstructural characteristics of dental amalgams

Metallographic studies by scanning electron microscopy and energy dispersive spectroscopy carried out for two types of dental amalgam showing a porous multiphase material. Surface analysis shows that the structure of the Dispersalloy amalgam consists of gamma-Ag3Sn, gamma(1)-Ag2Hg3, eta'-Cu6Sn5, epsilon-Cu3Sn and eutectic Ag-Cu phases. while Velvalloy amalgam consists mainly of gamma, gamma(1) and gamma(2)-Sn7-8Hg phases. The latter phase presents an uniform distribution often associated with voids.