Adsorption of heavy metal ions and epoxidation catalysis using a new polyhedral oligomeric silsesquioxane

The objective of this research was the preparation of a silsesquioxane functionalized with eight chloropropyl chains (T8-PrCl) and of a new derivative functionalized with a pendant linear chain (2-amino-1,3,4-thiadiazole - ATD; T8-Pr-ATD). The two nanostructured materials were characterized by 13C and 29Si NMR, FTIR and elemental analysis. The new nanostructured material, octakis[3-(2-amino-1,3,4-thiadiazole)propyl] octasilsesquioxane (T8-Pr-ATD), was tested as a ligand for transition-metal ions with a special attention to adsorption isotherms. The adsorption was performed using a batchwise process and the organofunctionalized surface showed the ability to adsorb the metal ions Cu (II), Co (II), and Ni (II) from water and ethanol. The adsorption isotherms were fitted by Langmuir, Freundlich, Temkin and Dubinin-Radushkevich (D-R) model. The kinetics of adsorption of metals were performed using three models such as pseudo-first order, pseudo-second order and Elovich. The Langmuir and Elovich models were the most appropriate to describe the adsorption and kinetic data, respectively. Furthermore, the T8-Pr-ATD was successfully applied to the analysis of environmental samples (river and sea water). Subsequently, a new nanomaterial was prepared by functionalization of the T8-Pr-ATD with a Mo (II) organometallic complex (T8-Pr-ATD-Mo). Only a few works in the literature have reported this type of substitution, and none dealt with ATD and Mo (II) complexes. The new Mo-silsesquioxane organometallic nanomaterial was tested as precursor in the epoxidation of cyclooctene and styrene. © 2012 Elsevier B.V.

Development of an electrochemical sensor based on nanostructured hausmannite-type manganese oxide for detection of sodium ions

The preparation and electrochemical characterization of hausmannite-type manganese oxide to use as a sensing material for sodium ion is described. This paper reports a new via synthetic to obtain of the hausmannite-type manganese oxide and its application in the construction of modified electrode as a voltammetric sensor. The electrochemical activity of hausmannite-type manganese oxide is controlled by intercalation/deintercalation of the sodium ions within the oxide lattice. The detection is based on the measurement of anodic current generated by oxidation of MnIII-MnIV at electrode surface. The best electrochemical response was obtained for a sensor composition of 20% (w/w) hausmannite oxide in the paste, a TRIS buffer solution of pH 6.0-7.0 and a scan rate of 50 mV s-1. A sensitive linear voltammetric response for sodium ions was obtained in the concentration range of 2.01 × 10 -5-2.09 × 10-4 mol L-1 with a slope of 355 μA L mmol-1 and a detection limit of 7.50 × 10 -6 mol L-1 using cyclic voltammetry. The use of hausmannite has significantly improved the selectivity of the sensor compared to the birnessite-type manganese oxide modified electrode. Under the working conditions, the proposed method was successfully applied to determination of sodium ions in urine samples. © 2013 Elsevier B.V.

Thermal behaviour of α-hydroxyisobutyric acid, sodium α-hydroxyisobutyrate and its compounds with some bivalent transition metal ions

Synthesis, characterization and thermal decomposition of bivalent transition metal α-hydroxyisobutyrates, M(C4H7O 3)2·nH2O (M = Mn(II), Fe(II), Co(II), Ni(II), Cu(II), Zn(II)), as well as the thermal behaviour of α-hydroxyisobutyric acid and its sodium salt were investigated employing simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), infrared spectroscopy (FTIR), TG-DSC coupled to FTIR, elemental analysis and complexometry. All the compounds were obtained as dihydrated, except the copper one which was obtained in the anhydrous state. The thermal decomposition of the anhydrous compounds occurs in a single or two steps and the final residue up to 235 C (Mn), 300 C (Fe), 305 C (Co), 490 C (Ni), 260 C (Cu) and 430 C (Zn) is Mn2O3, Fe2O3, Co3O 4, NiO, CuO and ZnO, respectively. The results also provided information concerning the ligand's denticity and identification of the gaseous products evolved during the thermal decomposition of these compounds. Copyright © 2013 Published by Elsevier B.V. All rights reserved.

Production, purification, and characterization of a major penicillium glabrum xylanase using brewer's spent grain as substrate

In recent decades, xylanases have been used in many processing industries. This study describes the xylanase production by Penicillium glabrum using brewer's spent grain as substrate. Additionally, this is the first work that reports the purification and characterization of a xylanase using this agroindustrial waste. Optimal production was obtained when P. glabrum was grown in liquid medium in pH 5.5, at 25 °C, under stationary condition for six days. The xylanase from P. glabrum was purified to homogeneity by a rapid and inexpensive procedure, using ammonium sulfate fractionation and molecular exclusion chromatography. SDS-PAGE analysis revealed one band with estimated molecular mass of 18.36 kDa. The optimum activity was observed at 60 °C, in pH 3.0. The enzyme was very stable at 50 °C, and high pH stability was verified from pH 2.5 to 5.0. The ion Mn2+ and the reducing agents β-mercaptoethanol and DTT enhanced xylanase activity, while the ions Hg2+, Zn2+, and Cu2+ as well as the detergent SDS were strong inhibitors of the enzyme. The use of brewer's spent grain as substrate for xylanase production cannot only add value and decrease the amount of this waste but also reduce the xylanase production cost. © 2013 Adriana Knob et al.

Synthesis, characterization and thermal behaviour of solid-state compounds of folates with some bivalent transition metals ions

Solid-state M-L compounds, where M stands for bivalent Mn, Co, Ni, Cu and Zn and L is folate (C19H17N7O6), have been synthesized. Simultaneous thermogravimetry and differential scanning calorimetry (TG-DSC), X-ray powder diffractometry, infrared spectroscopy (FTIR), TG-DSC coupled to FTIR, elemental analysis and high-resolution continuum source flame atomic absorption spectrometry technique (HR-CS FAAS) were used to characterize and to study the thermal behaviour of these compounds. The results provided information concerning the composition, dehydration, thermal stability and thermal decomposition. © 2013 Akadémiai Kiadó, Budapest, Hungary.

Solid-phase extraction of metal ions from fuel ethanol with a nanostructured adsorbent

This work describes the synthesis and characterization of a new octakis[3-(2,2'-dipyridylamine)propyl]octasilsesquioxane (T8-Pr-DPA), and a study of the metal ion preconcentration in fuel ethanol. Batch and column experiments were conducted to investigate for the removal of heavy metal ions from fuel ethanol. The results showed that the Langmuir allowed to describe the sorption equilibrium data of the metal ions on T8-Pr-DPA in a satisfactory way. The following maximum adsorption capacities (in mmolg-1) were determined: 3.62 for Fe (III), 3.32 for Cr (III), 2.15 for Cu (II), 1.80 for Co (II), 1.62 for Pb (II), 1.32 for Ni (II) and 0.88 for Zn (II). The thermodynamic parameters for the adsorption process such as free energy of adsorption (δG), enthalpy of adsorption (δH) and entropy of adsorption (δS) were calculated. Thermodynamic parameters showed that the system has favorable enthalpic, Gibbs free energy, and entropic values. The sorption-desorption of the metal ions has made possible the development of a preconcentration and determination method of metal ions at trace level in fuel ethanol. The method of quantitative analysis for Fe, Cu, Ni and Zn in fuel ethanol by Flame AAS was validated. Several parameters have been taken into account and evaluated for the validation of method, namely: linearity, limit of detection, limit of quantification, and the relative standard deviation and accuracy. The accuracy of the method was assessed by testing analyte recovery in the fuel ethanol samples. © 2013 Elsevier B.V.

Desenvolvimento de filtros solares a partir de complexos metálicos de Zn2+ e/ou Ce3+ com quercetina para protetores solares

Pós-graduação em Química - IQ

Passagens de ions peróxido para a superfície dentária externa após clareamento com peróxido de hidrogênio

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

O papel da argila na estabilização térmica de nanocompósitos: um estudo da ordem local e a média distância

Pós-graduação em Química - IQ

Purificação e caracterização bioquímica da α-glicosidase termoestável produzida por Thermoascus aurantiacus CBMAI 756

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

Purificação e caracterização bioquímica de poligalacturonases termoestáveis produzidas pelo fungo Thermoascus aurantiacus através de fermentação submersa e fermentação em estado sólido

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

Produção, isolamento e caracterização de 'beta'-galactosidades de Trichoderma reesei: interação de íons metálicos na atividade enzimática

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Verres et vitrocéramiques à base de chalco: halogénures dopés par des ions de terres rares pour la luminescence dans le visible

Pós-graduação em Química - IQ

Evaluation of the electrochemical behavior of carbon paste electrode (CPE) with chalcopyrite (CuFeS2) in the presence of ferrous ions

In this work we present an electrochemical study using carbon paste electrode (CPE) with CuFeS2 in solutions with different concentrations of Fe2+ ions in order to evaluate the possible interaction between these ions and mineral sulfide in the absence and presence of the bacteria Acidithiobacillus ferroxidans.

Thermal behaviour of nicotinic acid, sodium nicotinate and its compounds with some bivalent transition metal ions

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