Synthesis, characterization and thermal behavior of complexes of Cu(II), Zn(II) and Cd(II) with S,S '-methylenebis(cysteine)

Synthesis and characterization, including data on thermal decomposition, are reported for the complexes of S,S'-methylenebis(cysteine) (djenkolic acid) with copper(II), zinc(II) and cadmium(II): CuC(7)H(12)N(2)O(4)S(2) [I]; ZnC(7)H(12)N(2)O(4)S(2) [II] and CdC(7)H(12)N(2)O(4)S(2) [III] X-ray diffraction showed that the compounds are isostructural and belong to a monoclinic system. According to IR spectra, COO, NH(2) groups and bridging sulfur atoms are the main coordination sites.

In situ and simultaneous nanostructural and spectroscopic studies of ZnO nanoparticle and Zn-HDS formations from hydrolysis of ethanolic zinc acetate solutions induced by water

The simultaneous formation of nanometer sized zinc oxide (ZnO), and acetate zinc hydroxide double salt (Zn-HDS) is described. These phases, obtained using the sol-gel synthesis route based on zinc acetate salt in alcoholic media, were identified by direct characterization of the reaction products in solution using complementary techniques: nephelometry, in situ Small-Angle X-ray Scattering (SAXS), UV-Vis spectroscopy and Extended X-ray Absorption Fine Structures (EXAFS). In particular, the hydrolytic pathway of ethanolic zinc acetate precursor solutions promoted by addition of water with the molar ratio N = [H2O]/[Zn2+] = 0.05 was investigated in this paper. The aim was to understand the formation mechanism of ZnO colloidal suspension and to reveal the factors responsible for the formation of Zn-HDS in the final precipitates. The growth mechanism of ZnO nanoparticles is based on primary particle (radius approximate to 1.5 nm) rotation inside the primary aggregate (radius < 3.5 nm) giving rise to an epitaxial attachment of particles and then subsequent coalescence. The growth of second ZnO aggregates is not associated with the Otswald ripening, and could be associated with changes in equilibrium between solute species induced by the superficial etching of Zn-HDS particles at the advanced stage of kinetic.

SURFACE EFFECTS IN THE HYDROGEN EVOLUTION REACTION ON NI-ZN ALLOY ELECTRODES IN ALKALINE-SOLUTIONS

Hydrogen evolution reaction was studied on Ni-Zn (25% of Ni before leaching) in 1 M NaOH at 25 degrees C. These electrodes were characterized by very low Tafel slopes of 67 mV dec(-1). Other techniques used included potential and current pulse, potential relaxation in an open circuit, and ac impedance spectroscopy. Analysis of the experimental results led to the conclusion that hydrogen adsorption in the surface layers was responsible for the observed behavior. Influence of the oxidation of the electrode surface and the addition of poisons, thiourea and cyanides, were also studied. These processes inhibit the hydrogen absorption and restore ''normal'' Tafel slopes. Kinetic parameters of the hydrogen evolution reaction were determined.

Paper-based diffusive gradients in thin films technique coupled to energy dispersive X-ray fluorescence spectrometry for the determination of labile Mn, Co, Ni, Cu, Zn and Pb in river water

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

Determination of Ca, Mg, and Zn in biodiesel microemulsions by FAAS using discrete nebulization

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

Adsorption of MX2 (M = Mn, Ni, Cu, Zn, and Cd; X = Cl, Br, and I) and FeCl3 by modified silica surface with imidazolylpropyl group

Silica gel surface modified with imidazolylpropyl group was used to adsorb MX2 (M = Mn, Ni, Cu, Zn, and Cd; X = Cl, Br, and I) and FeCl3 from ethanol and acetone solution. The adsorption capacity and the intensity of the adsorption were determined by using the Langmuir equation. The influences of the solvent, temperature, and degree of functionalization on the adsorption were also studied. The infrared spectra of the functionalized silica were recorded between 1700-1300 cm-1. The bands of the imidazole skeletal vibrations are shifted to higher frequencies upon metal-to-base nitrogen interaction. © 1985.

Adsorption of Cu(II), Zn(II), Cd(II), Hg(II) and Pb(II) from aqueous solutions on a 2-mercaptobenzimidazole-modified silica gel

The chemically modified silica, obtained by reacting 2-mercaptobenz-imidazole with 3-chloropropyl silica gel, was used to adsorb Cu(II), Zn(II), Cd(II) and Pb(II) from aqueous solutions at various pH. Between pH 3-5, the order of selectivity was Hg(II) > Cd(II) ≫ Cu(II) ∼ Zn(II) ∼ Pb(II). Under batch conditions retentions of 100% were achieved for all metals except for Pb(II) where 93% was attained. Under column conditions recoveries of 100% were obtained for all metals. © 1990 Springer-Verlag.

Influence of the heat treatment in the electrochemical corrosion of Al-Zn-Mg alloys

The localized corrosion of Al-(5.03%)Zn-(1.67%)Mg-(0.23%)Cu alloys and high purity Al has been studied using electrochemical techniques, optical microscopy, SEM and EDX. The samples were previously submitted to different heat treatments in which coherent and incoherent MgZn 2 precipitates with different distribution and aggregation degree were produced. The influence of NaCl and Na 2SO 4, dissolved oxygen, immersion time and convection were studied. In NaCl solutions, pitting potentials for the alloys were more negative than for aluminium, indicating an increase in their susceptibility to localized corrosion. Moreover, annealed and cold-rolled alloys presented more negative pitting and repassivation potentials than those submitted to age hardening with direct or interrupted quenching. In annealed and cold-rolled samples, pit nucleation and propagation takes place in the zones where MgZn 2 is accumulated. In the case of the age-hardened alloys, a double pitting behaviour is observed, the first one in the magnesium and zinc enriched regions and the second in the matrix. While the cold water quenched alloy is susceptible to stress corrosion craking, the alloy submitted to the interrupted quenching process is less susceptible to intergranular attack. The sulphate ion shifts the pitting potential of aluminium and the alloys by chloride towards more positive values because it impedes local accumulations of the latter. © 1992 Chapman & Hall.

A simple method based on HR-CS FAAS for multi-element determination of Cu, Fe, Mn and Zn in medicinal plants

A simple method to determine Cu, Fe, Mn and Zn in single aliquots of medicinal plants by HR-CS FAAS is proposed. The main lines for Cu, Mn and Zn, and the alternate line measured at the wing of the main line for Fe at 248.327 nm allowed calibration within the 0.025 - 2.0 mg L-1 Cu, 1.0 - 20.0 mg L-1 Fe, 0.05 - 2.0 mg L-1 Mn, 0.025 - 0.75 mg L-1 Zn ranges. Nineteen medicinal plants and two certified plant reference materials were analyzed. Results were in agreement at a 95% confidence level (paired t-test) with reference values. Limits of detection were 0.12 μg L-1 Cu, 330 μg L-1 Fe, 1.42 μg L-1 Mn and 8.12 μg L-1 Zn. Relative standard deviations (n=12) were ≤ 3% for all analytes. Recoveries in the 89 - 105% (Cu), 95 - 108% (Fe), 94 - 107% (Mn), and 93 - 110% (Zn) ranges were obtained.

Concentrations of Cu, Fe, Mn, and Zn in tropical soils amended with sewage sludge and composted sewage sludge

Sewage sludge may be used as an agricultural fertilizer, but the practice has been criticized because sludge may contain trace elements and pathogens. The aim of this study was to compare the effectiveness of total and pseudototal extractants of Cu, Fe, Mn, and Zn, and to compare the results with the bioavailable concentrations of these elements to maize and sugarcane in a soil that was amended with sewage sludge for 13 consecutive years and in a separate soil that was amended a single time with sewage sludge and composted sewage sludge. The 13-year amendment experiment involved 3 rates of sludge (5, 10, and 20 t ha-1). The one-time amendment experiment involved treatments reflecting 50, 100, and 200 % of values stipulated by current legislation. The metal concentrations extracted by aqua regia (AR) were more similar to those obtained by Environmental Protection Agency (EPA) 3052 than to those obtained by EPA3051, and the strongest correlation was observed between pseudo(total) concentrations extracted by AR and EPA3052 and bioavailable concentrations obtained by Mehlich III. An effect of sewage sludge amendment on the concentrations of heavy metals was only observed in samples from the 13-year experiment. © 2012 Springer Science+Business Media B.V.

Associação entre composição corporal, equilíbrio e mobilidade de idosos com 80 anos ou mais

Study design: cross-sectional study. Objective: The objective of this study was to analyze the association between body composition, mobility and balance of elderly aged 80 years or older. Methods: The sample consisted of 123 elderly aged 80 and 95 years (83.2 ± 2.7 years) with 78 women (83.2 ± 2.9 years) and 45 men (83.2 ± 2, 4 years) residing in the city of Presidente Prudente - SP. Assessment of body composition was made by absorpiometria dual energy X-ray (DXA). The mobility and balance were assessed by means of tests of speed walking, and static balance lower limb strength. For statistical analysis we carried out the chi-square test, the software used was SPSS (13.0) and the significance level was set at 5%. Results: In males, those with higher performance in the functional tests showed higher percentages of muscle mass (MM) (35.6%) compared to lower performance (15.6%), p = 0.026. In the female group, the elderly with higher performance on tests showed higher bone mineral density (BMD) values (30.8%) compared with those with lower performance (20.5%) p = 0.041. Conclusion: MM for elderly males and BMD for females were the components of body composition that is associated with functional capacity.

Testing extractants for Cu, Fe, Mn, and Zn in tropical soils treated with sewage sludge for 13 consecutive years

In this paper, we report on a field experiment being carried out in a Typic Eutrorthox. The experiment was initiated in the 1997-98 agricultural season as a randomized block design with four treatments (0, 5, 10, and 20 t ha -1) of sewage sludge and five replicates. Compound soil samples were obtained from 20 subsamples collected at depths of 0-0.1 and 0.1-0.2 m. Cu, Fe, Mn, and Zn concentrations were extracted with DTPA pH 7.3; 0.1 mol L -1 HCl, Mehlich-I, Mehlich-III, and 0.01 mol L-1 CaCl 2. Metal concentrations were determined via atomic absorption spectrometry. Diagnostic leaves and the whole above-ground portion of plants were collected to determine Cu, Fe, Mn, and Zn concentrations extracted by nitric-perchloric digestion and later determined via atomic absorption spectrometry. Sewage sludge application caused increases in the concentrations of soil Cu, Fe, and Mn in samples taken from the 0-0.1 m depth evaluated by the extractants Mehlich-I, Mehlich-III, 0.01 mol L-1 HCl and DTPA pH 7.3. None of the extractants provided efficient estimates of changes in Mn concentrations. The acid extractants extracted more Cu, Fe, Mn, and Zn than the saline and chelating solutions. The highest concentrations of Cu, Fe, and Zn were obtained with Mehlich-III, while the highest concentrations of Mn were obtained with HCl. We did not observe a correlation between the extractants and the concentrations of elements in the diagnostic leaves nor in the tissues of the whole maize plant (Zea mays L.). © 2013 Springer Science+Business Media Dordrecht.

Role of Ca, Fe, Cu and Zn in breast cancer: Study by X-ray fluorescence techniques and immunohistochemical analysis

In recent years, several studies have shown that concentrations of trace elements are altered in neoplastic breast tissues. However, the microenvironment and metabolic changes caused by tumors are complex and still not completely understood. Under this aspect, the combination of different techniques to investigate the role of trace elements in promoting and/or maintaining a tumor is interesting once the combination of information obtained by analytical techniques and immunohistochemical assays, associated with clinicopathological data, may allow a better metabolic understanding of trace elements in breast cancer. In this work, the role of the trace elements Ca, Fe, Cu and Zn in neoplastic breast tissues was investigated by X-ray fluorescence (XRF) techniques and immunohistochemical assays. We determined concentrations of Ca, Fe, Cu and Zn in normal and neoplastic breast tissues using energy dispersive XRF, and these values were used to set the positive or negative expression of elements in normal and neoplastic tissues. These expressions were correlated with the spatial distributions of trace elements (evaluated by micro-XRF) and with immunoexpression of matrix metalloproteinases (MMPs), tissue inhibitors of MMPs and vascular endothelial growth factor. The results revealed that the expression of the trace elements Fe, Cu and vascular endothelial growth factor are related, indicating that higher levels of these elements can be associated with the angiogenic process in breast cancer. Also, associations between Ca, Zn and MMPs expression have been observed, possibly because of the fact that both metals are present in these proteins. © 2013 John Wiley & Sons, Ltd.