Desenvolvimento de uma metodologia para determinação de Pb2+ em matrizes aquosas utilizando nanopartículas magnéticas

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Universidade Federal de Goiás


The iron oxide (Fe3O4) nanoparticles are promising adsorbents and, in this work, they were synthesized, characterized and applied as adsorbents in the adsorption of lead ions (Pb2+) using solid phase magnetic extraction (MSPE). The iron oxide was synthesized by the coprecipitation method and the obtained nanoparticles presented the crystalline phase of the oxide, being proved by the characterization by X-Ray Diffraction, X-ray Dispersive Energy and Absorption Spectroscopy in the Infrared region. In order to obtain information on the surface charge of the synthesized material, the pH at the zero loading point (pHPCZ) was determined indicating that the oxide surface is negatively charged at pH values above 9.4. Once the best pH (9.0) for adsorption was defined, the influence of the variables agitation time and mass of the adsorbent were evaluated, fixing them in 4 min and 3.0 mg respectively, in order to obtain the best conditions of the adsorption. adsorption process. The maximum adsorption capacity was obtained by the construction of adsorption isotherms, and a value of 31.60 mg.g1 was found. Through the kinetic study, it was observed that the adsorption obeys a pseudo-first-order kinetics. After the adsorption was optimized, the best desorption parameters were evaluated, aiming the development of an extraction/preconcentration method. Thus, 500μL of 0.5 mol.L-1 nitric acid was used as the eluent. The analytical performance was evaluated by means of the parameters, limit of detection (L.D.), limit of quantification (L.Q.), precision (D.P.R) and values found were 5.44 μg.L-1 ; 16.48 μg.L-1 and 0.25%, respectively, with the linear range of the method being 16.48 -500 μg.L-1 . Finally, the accuracy of the method was evaluated from recovery tests on samples of mineral water, micellar water and facial makeup with recovery values in the range of 95.94 - 118%. In addition, analyzes of certified water reference material (APS-1071) were also made to verify the accuracy of the proposed method.



Óxidos de ferro, Extração magnética em fase sólida, Chumbo, Adsorção, Iron oxides, Solid phase magnetic extraction, Lead, Adsorption


SILVA, C. A. S. Desenvolvimento de uma metodologia para determinação de Pb2+ em matrizes aquosas utilizando nanopartículas magnéticas. 2018. 83 f. Dissertação (Mestrado em Química) - Universidade Federal de Goiás, Catalão, 2018.