Síntese, caracterização e estudo do comportamento térmico dos 2-metoxibenzoatos de lantanídeos no estado sólido

Foram sintetizados no estado sólido os compostos Ln-2-MeO-Bz, sendo que Ln representa os lantanídeos trivalentes e Y (III) e 2-MeO-Bz representa o 2-methoxibenzoato. Os compostos foram sintetizados por adição estequiométrica, sob agitação, do ligante nas respectivas soluções de cloretos ou nitratos de lantanídeos. A precipitação dos compostos só ocorreram quando as soluções foram parcialmente evaporadas em banho maria. A caracterização dos compostos foi realizada utilizando-se de métodos convencionais: difratometria de raios X pelo método do pó, espectroscopia de absorção na região do infravermelho, análise elementar e as técnicas termoanalíticas TG/DTG (termogravimetria / termogravimetria derivada simultânea) e TG – DTA (termogravimetria - análise térmica diferencial simultânea) e DSC (Calorimetria exploratória diferencial). Estas técnicas puderam dar informações sobre desidratação, modos de coordenação, comportamento térmico, estequiometria e estrutura dos compostos sintetizados. Com os resultados das curvas TG e da complexometria, pôde-se estabelecer a fórmula geral de cada composto sintetizado. Pela análise dos difratogramas de raios X foi observado que todos os compostos sintetizados são cristalinos e que os compostos de lutécio e itérbio são isomorfos. A observação dos espectros de infravermelho teórico e experimental sugerem uma coordenação bidentada sem equalização de cargas entre o 2-metoxibenzoato e os seus respectivos centros metálicos. As curvas TG-DTA e DSC forneceram informações inéditas e importantes sobre o comportamento e a decomposição térmica dos compostos sintetizados.Solid state Ln 2-MeO-Bz compounds, where Ln stands for trivalent La to Lu and Y (III) and 2-MeO-Bz is 2-methoxybenzoate, have been synthesized. The solid state compounds were prepared by stoichiometric relation adding slowly, with continuous stirring the ligand solution to the respective metal chloride or nitrate solutions. No precipitate was observed during the addition of sodium 2-methoxybenzoate; however the precipitate was obtained when the solution was evaporated in a water bath. Simultaneous thermogravimetry and differential thermal analysis (TG-DTA), differential scanning calorimetry (DSC), X-ray powder diffraction, infrared spectroscopy, elemental analysis and complexometry, were used to characterize and to study the thermal behaviour of these compounds. The results led to information about composition, dehydration, coordination mode, structure, thermal behaviour and thermal decomposition of the isolated compounds. From TG curves and complexometry results, a general formula could be established for these compounds in the solid state. The X-ray powder patterns pointed out that the synthesized compounds have a crystalline structure without evidence concerning to the formation of isomorphous series, except the ytterbium and lutetium compounds. The experimental and theoretical infrared spectroscopy data suggest that 2-metoxibenzoate acts as a bidentate bond with an incomplete equalization of bond lenghts in the carboxylate anion. The TG-DTA and DSC curves provided previously unrerported information concerning the thermal behaviour and thermal decomposition of these compounds.Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES

Thermal and spectroscopic study of the 3,4-(methylenedioxy) cinnamate compounds of transition metals in the solid state

In this study, the trans-3,4-(methylenedioxy)cinnamic acid was used as precursor for the synthesis of transition metal compounds, which were characterized by coupled TG-DTA/FT-IR system, elemental analysis, FT-IR spectroscopic study and titrimetric analysis with EDTA. The characterization by these techniques allowed to determine the hydration water content, number of ligand coordinated to the metal, thermal behavior and thermal stability, as well as monitor the main gaseous products released in each decomposition step. The elemental and titrimetric analyses were performed in order to support TG-DTA data. A theoretical FT-IR calculation was made using the Gauss View 5.0.2 W program and the vibration frequencies obtained were compared with the experimental ones showing as a result a difference of around 30 cm(-1) between them. In these spectra were analyzed the main vibration modes as COO- (carboxylate group), -C=C- (aromatic ring, alkene), -C-O- and -CH2 (methylenedioxy group) and -C-H (alkenes, aromatic). (C) 2014 Elsevier B.V. All rights reserved.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

Ibuprofen biosorption by chemically activated Saccharomyces cerevisiae

Saccharomyces cerevisiae biomass was activated chemically, and its ibuprofen (IBP) biosorption capabilities were assessed regarding IBP removal from an aqueous solution. The effects of pH (2-10), contact time (0-90 min), IBP concentration (5-35 mg L-1), and temperature (20, 30, 40°C) were evaluated in batch studies. Higher removal rates of IBP were found at pH 2.0. The pseudo-second-order kinetic model best described the experimental data. Both the Langmuir and Freundlich isotherm models described the equilibrium data satisfactorily. The maximum biosorption capacity for IBP onto chemically activated Saccharomyces cerevisiae biomass (CA-YB) was estimated at 13.39 mg g-1 at 40°C. The activation energy calculated by the Dubinin-Radushkevich isotherm model was 9.129 kJ mol-1, indicating that a chemical process mediated the biosorption of IBP onto CA-YB. According to thermodynamic studies, IBP biosorption is spontaneous and endothermic. FTIR analysis revealed that the carboxyl, hydroxyl, phosphoryl, and amino groups were involved in the biosorption process of IBP. These findings indicated that CA-YB could be an alternative biosorbent for IBP removal from aqueous media