Teses em Química (Doutorado) - PPGQ/ICEN

URI Permanente para esta coleçãohttps://repositorio.ufpa.br/handle/2011/4047

O Doutorado Acadêmico pertence ao Programa de Pós-Graduação em Química (PPGQ) do Instituto de Ciências Exatas e Naturais (ICEN) da Universidade Federal do Pará (UFPA).

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Acesso aberto (Open Access)
Estudo de eletrocatalisadores de PtRu, PtRuRh e PtRuPd obtidos por modificação no Método Borohidreto de Sódio para eletro-oxidação de metanol e etanol
(Universidade Federal do Pará, 2016-01-25) ANDRADE, Flávio Vargas; SOUZA, José Pio Iúdice de; http://lattes.cnpq.br/1448978342555218
PtRu, PtRuRh and PtRuPd electrocatalysts supported on carbon has been widely studied for electro-oxidation of methanol and ethanol. Among different possibilities of preparing these electrocatalysts is the method of reducing with sodium borohydride. For the catalytic activity is optimized, it is necessary that the electrocatalyst is distributed evenly. One possibility is the use of complex precursor salts, including those with amine linker. In this work, we tried to assess the effect of adding an ammonium hydroxide solution (NH4OH) the solution of precursors. The electrocatalysts were characterized physically by Transmission Electron Microscopy (TEM), Energy Dispersive X-ray (EDX) and X-ray diffraction (XRD). For the electrochemical characterization, the techniques of chronoamperometry and cyclic voltammetry were used. The results of EDX showed that the compositions of the electrocatalysts were very close to the nominal composition. The crystallite size and the lattice parameter obtained by XRD showed changes with the change of the method. The TEM results show a homogeneous distribution more particle on electrocatalysts preparations with the addition of NH4OH solution 4 mol L-1 although this is not be determinant in electrocatalytic activity. Nos electrochemical testicles, as chains were for standard electro-oxidation of CO and load monolayer for the mass activity and compared this way. The cyclic voltammetry and chronoamperometry results showed different activities paragraph an electro-oxidation of methanol and ethanol. The results of DEMS electrocatalysts trimetallic of PtRuRh and PtRuPd showed different amounts of products and volatile. This way possible and establish an activity order these electrocatalysts.
Acesso aberto (Open Access)
Técnicas voltamétricas com eletrodo de filme de bismuto modificado com edta e ebt para determinação de Ca2+ e Mg2+ em biodiesel
(Universidade Federal do Pará, 2016-08-19) MULLER, Renata Medeiros Lobo; MARQUES, Aldalea Lopes Brandes; http://lattes.cnpq.br/0121030502015990; MÜLLER, Regina Celi Sarkis; http://lattes.cnpq.br/654941494386147
This study presents the development of alternative electrochemical methods for the determination of Mg2+ and Ca2+ through voltammetry technique of adsorptive stripping voltammetry (VAdR) with anodic scan. Bismuth film electrode modified with eriochrome black-T (EBT) was used for modification of the electrode in the determination of Mg2+ in the pulse differential mode (DPAdSV), while EDTA has been used for determination of Ca2+ in wave mode square (SWAdSV). The determination of Mg2+ was performed using acetate buffer (0.1 mol L-1) at pH = 4.5, EBT as supporting electrolyte and 1.0 x 10-3 mol L-1 as a binder. Successive additions of aliquots of the stock solution were made Mg2+ 1.0 x 10-3 mol L-1 so that the ion was pre-concentrated on the sensor surface under the following conditions optimized voltammetric: deposition potential (EDEP) = - 1.0 V; Pre time - concentration (Tpre) = 120 s; scan speed (v) = 0.050 V s-1; pulse amplitude (Amp) = 0.1 V. The complex formed Mg2+ EBT showed a peak current of about - 0.6 V. The determination of Ca2+ was made using ammonium buffer (0.01 mol L-1) at pH 9.4, as supporting electrolyte and EDTA 1.0 x 10-2 mol L-1 as a binder under the following optimum conditions: deposition potential (EDEP) = -1.0 V; preconcentration time (Tpre) = 90 sec; frequency (freq.) = 15 Hz; width = 0,075V and Step E) = 0.004 V. The complex formed Ca2+ EDTA showed a peak current of approximately - 0.2 V. The result was consistent statistically considering t -test for a 95% confidence level. The levels were lower CV of 11.0% (Mg2+ and Ca2+), recoveries were in the range 95.0 to 108.0% (Mg2+) and from 97.8 to 105.0% (Ca2+) and the values of detection limits were 1.05 x 10-6 mol L-1 (Mg2+) and 2.8 x 10-7 mol L-1 (Ca2+), and quantitation 3.51 x 10-6 mol L-1 (Mg2+) and 9.46 x 10-7 mol L-1 (Ca2+) for the samples analyzed, showing good accuracy and sensitivity of the proposed method. The values obtained for the samples ranged from 1.47 x 10-5 ± 1.28 x 10-6 mol L-1 (Mg2+) and 5.57 x 10-6 ± 3.77 x 10-7 mol L-1 (Ca2+) on samples of biodiesel. The determination of metals such as Ca2+ and Mg2+ by electrochemical techniques with chemically modified electrodes has as main advantages its detectability and the selectivity.

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