Browsing by Author "Fraceto, Leonardo Fernandes"
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Item Approach combining on-line metal exchange and tangential-flow ultrafiltration for in-situ characterization of metal species in humic hydrocolloids.(2010) Goveia, Danielle; Lobo, Fabiana Aparecida; Burba, Peter; Fraceto, Leonardo Fernandes; Dias Filho, Newton Luiz; Rosa, André HenriqueThis paper deals with the development and optimization of an analytical procedure using ultrafiltration and a flow-injection system, and its application in in-situ experiments to characterize the lability and availability of metal species in humic-rich hydrocolloids. The on-line system consists of a tangential flow ultrafiltration device equipped with a 3-kDa filtration membrane. The concentration of free ions in the filtrate was determined by atomic-absorption spectrometry, assuming that metals not complexed by aquatic humic substances (AHS) were separated from the complexed species (M–AHS) retained by the membrane. For optimization, exchange experiments using Cu(II) solutions and AHS solutions doped with the metal ions Ni(II),Mn(II), Fe(III), Cd (II), and Zn(II) were carried out to characterize the stability of the metal–AHS complexes. The new procedure was then applied in-situ at a tributary of the Ribeira do Iguape river (Iguape, São Paulo State, Brazil) and evaluated using the ions Fe(III) and Mn(II), which are considered to be essential constituents of aquatic systems. From the exchange between metal–natural organic matter (M–NOM) and the Cu(II) ions it was concluded that Cu(II) concentrations >485 μg L−1 were necessary to obtain maximum exchange of the complexes Mn–NOM and Fe–NOM, corresponding to 100% Mn and 8% Fe. Moreover, the new analytical procedure is simple and opens up new perspectives for understanding the complexation, transport, stability, and lability of metal species in humic-rich aquatic environments.Item Desenvolvimento de nanocápsulas de poli-e-caprolactona contendo o herbicida atrazina.(2012) Souza, Patrícia Moraes Sinohara; Lobo, Fabiana Aparecida; Rosa, André Henrique; Fraceto, Leonardo FernandesIn this study, polymeric nanocapsules of PCL containing the herbicide atrazine were prepared. In order to optimize the preparation conditions, a 23 factorial design was performed using different formulations of nanocapsules, which investigated the influence of three variables at two levels. The factors varied were the quantities of PCL, Span 60 and Myritol. The results were evaluated considering the size, polydispersity, zeta potential and association rate and the measures of these parameters were taken immediately after preparation and after 30 days of preparation. The formulations with minimum level of polymer in the preparation showed better stability results.Item Development of a method to determine Ni and Cd in biodiesel by graphite furnace atomic absorption spectrometry.(2011) Lobo, Fabiana Aparecida; Goveia, Danielle; Oliveira, Adriana Paiva de; Romão, Luciane Pimenta Cruz; Fraceto, Leonardo Fernandes; Dias Filho, Newton Luiz; Rosa, André HenriqueThis paper proposes a low cost, simple, fast method for determining Ni and Cd in biodiesel samples by graphitefurnaceatomicabsorptionspectrometry (GFAAS). The method was evaluated in biodiesel from different sources. Tungsten was used as a permanent modifier and the samples were prepared in the form of microemulsions, by mixing about 0.5 g of biodiesel with 5 g of surfactant (Triton X-100) in volumetric flasks and completing the volume with HNO3 1% (v/v). The detection limits obtained for Ni and Cd in microemulsions were ≤0.9 and 0.1 μg L−1, respectively. The relative standard deviation (% R.S.D., n = 12) was ≤8.20% for Ni (washed animal fat sample) and ≤4.71% for Cd (sunflower oil sample). Accuracy was checked based on addition and recovery experiments, which yielded recovery rates varying from 93% to 108% for Ni and from 98% to 116% for Cd. Sample preparation is rapid and easy, and the use of an inorganic standard for calibration makes this sample preparation procedure suitable for routine applications.Item Poly(hydroxybutyrate-co-hydroxyvalerate) microspheres loaded with atrazine herbicide : screening of conditions for preparation, physico-chemical characterization, and in vitro release studies.(2011) Lobo, Fabiana Aparecida; Aguirre, Carina Levy de; Silva, Mariana Santos; Grillo, Renato; Melo, Nathalie Ferreira Silva de; Oliveira, Liliam Karla de; Morais, Leandro Cardoso de; Campos, Valquíria; Rosa, André Henrique; Fraceto, Leonardo FernandesDue to their widespread use in agriculture as well as in urban areas, agricultural chemicals are globally some of the most commonly encountered substances in waters. The objective of this study is to develop (including preparation and characterization) a new modified release system for the herbicide atrazine, employing poly(hydroxybutyrate-co-hydroxyvalerate) (PHBV) microspheres. The microspheres were prepared by the emulsification/solvent evaporation method, emulsifying an organic phase (atrazine and PHBV dissolved in chloroform) into an aqueous phase containing polyvinyl alcohol (PVA) as surfactant, under stirring, and then evaporating the solvent. A 24-1 fractional factorial design, investigating the influence of four variables at two levels, was performed to obtain formulations with optimized association efficiencies. There was a greater dependence of association efficiency on PVA concentration (negative) and the mass of polymer (positive) with lesser influence of both stirring speed and organic phase volume. The size of the particles was assessed using scanning electron microscopy, which showed that the particles were rough-surfaced spheres. The results obtained are promising, since the formulations presented encapsulation efficiency near 25% and the release kinetics profile of atrazine was altered when it was encapsulated in the microparticles, indicating that these systems may be efficient in reducing the environmental impact caused by the herbicide, hence making it safer to use.Item Polymeric microparticles for modified release of NPK in agricultural applications.(2018) Chagas, Júnior Olair; Gomes, José Messias; Cunha, Isabela Cristina de Matos; Melo, Nathalie Ferreira Silva de; Fraceto, Leonardo Fernandes; Silva, Gilmare Antônia da; Lobo, Fabiana AparecidaThe aim of this work was to synthesize polymeric microparticles as carriers for nitrogen, phosphorus, and potassium (NPK fertilizer) for agricultural applications, using polyglycerol (PG) to improve the synthesis procedure. Multivariate experimental designs were employed to obtain a satisfactory synthesis. The desirability function identified the best conditions for preparation of the microparticles as being 100.00 mg of poly(e-caprolactone) (PCL), 825.00 mg of PG, 9.25 mL of chloroform, and 0.9% w/v of polyvinyl alcohol (PVA). This resulted in average encapsulation rates of 94.23% for N, 99.80% for P, and 65.00% for K. The profile of release from the microparticles was according to diffusion following Fick’s Law. These observations confirmed the capacity of the proposed microparticles to sustain a continuous and prolonged release of NPK for the purpose of plant fertilization.Item Preparação de membranas de acetato de celulose organomodificadas para adsorção dos íons Cu(II), Cd(II), Mn(II) E Ni(II).(2010) Goveia, Danielle; Lobo, Fabiana Aparecida; Rodrigues Filho, Ubirajara Pereira; Dias Filho, Newton Luiz; Fraceto, Leonardo Fernandes; Rosa, André HenriqueCellulose acetate polymeric membranes had been prepared by a procedure of two steps, combining the method of phase inversion and the technique of hydrolysis-deposition. The first step was the preparation of the membrane, and together was organomodified with tetraethylortosilicate and 3-aminopropyltrietoxysilane. Parameters that exert influence in the complexation of the metallic ion, as pH, time of complexation, metal concentration, had been studied in laboratory using tests of metal removal. The membranes had presented resistance mechanics and reactivity to cations, being able to be an alternative for the removal, daily pay-concentration or in the study of the lability of metals complexed.