DISSERTAÇÃO DE MESTRADO - PROGRAMA DE PÓS-GRADUAÇÃO EM QUIMICA

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    Um novo e seletivo sensor à base de CuTSPc e óxido de grafeno reduzido para a determinação individual e simultânea dos antioxidantes BHA e TBHQ em amostras de biodiesel
    (Universidade Federal do Maranhão, 2016-07-29) Carvalho, Rita Maria de Sousa; LUZ, Rita de Cássia Silva; 812.848.293-91
    A novel and selective electrochemical sensor for the determination of the butylated hydroxyanisole (BHA) and tert-butylhydroquinone (TBHQ) antioxidants employing the differential pulse voltammetry (DPV) was developed. In this sense, a glassy carbon electrode (GCE) modified with a copper tetrasulfonated phthatocyanine (CuTSPc) adsorbed on reduced graphene oxide (rGO) showed excellent response for the TBHQ and BHA oxidation with a decrease in the overpotentials about 130mV vs Ag/AgCl and anodic peak currents about 4 times higher than the observed responsesat an electrode unmodified. The increase of the oxidation reaction rates for TBHQ and BHA was attributed to the efficient electron transfer between the studied species and the immobilized materials on surface of the GCE.The materials rGO, CuTSPc and rGO/CuTSPc were characterized by Fourier transform infrared spectroscopy (FTIR) and the analytical response of the sensor for the analytes was studied by cyclic voltammetry (CV) and linear scan voltammetry (LSV) techniques. After optimization of the experimental parameters, the analytical curves for determination of BHA and TBHQ by DPV technique demonstrated an excellent linear response from 0.1 to 500µmol L-1 with detection limit of 0.045 µmol L-1 for TBHQ and 0.036 µmol L-1 for BHA. Finally, the proposed method was successfully applied in the simultaneous determination of BHA and TBHQ in six biodiesel samples, and the results obtained were found to be similar to those obtained using the HPLC method with agreement at 95 % confidence level. The addition and recovery studies have shown that the proposed method has good accuracy with recovery values between 99.5 and 100.5 % forTBHQ and 99.1 and 100.2 for BHA.