Magister Scientiae - MSc (Chemistry) / Electrochemical platforms were developed based on pencil graphite electrodes (PGEs) modified electrochemically with reduced graphene oxide metal nanoparticles (ERGO-metalNPs) composite and used for the high-sensitivity determination of Bisphenol A (BPA) in water samples. Synergistic effects of both reduced Graphene Oxide sheets and metal nanoparticles on the performance of the pencil graphite electrode (PGE) were demonstrated in the oxidation of BPA by differential pulse voltammetry (DPV). A solution of graphene oxide (GO) 1 mg mL-1 and 15 ppm of metal stock solutions (1,000 mg L-1, atomic absorption standard solution) (Antimony or Gold) was prepared and after sonication deposited onto pencil graphite electrodes by cyclic voltammetry reduction. Different characterization techniques such as FT-IR, HR-SEM, XRD and Raman spectroscopy were used to characterize the GO and ERGO-metalNPs. Parameters that influence the electroanalytical response of the ERGO-SbNPs and ERGO-AuNPs such as, pH, deposition time, deposition potential, purging time were investigated and optimized. Well-defined, reproducible peaks with detection limits of 0.0125 ?M and 0.062 ?M were obtained for BPA using ERGO-SbNPs and ERGO-AuNPs respectively. The rGO-metalNPs-PGE was used for the quantification of BPA in tap water sample and proved to be suitable for the detection of BPA below USEPA prescribed drinking water standards of 0.087 ?M. / 2021-12-31

Magister Scientiae - MSc (Chemistry) / Electrochemical platforms were developed based on pencil graphite electrodes (PGEs) modified electrochemically with reduced graphene oxide metal nanoparticles (ERGO–metalNPs) composite and used for the high-sensitivity determination of Bisphenol A (BPA) in water samples. Synergistic effects of both reduced Graphene Oxide sheets and metal nanoparticles on the performance of the pencil graphite electrode (PGE) were demonstrated in the oxidation of BPA by differential pulse voltammetry (DPV). A solution of graphene oxide (GO) 1 mg mL-1 and 15 ppm of metal stock solutions (1,000 mg L-1, atomic absorption standard solution) (Antimony or Gold) was prepared and after sonication deposited onto pencil graphite electrodes by cyclic voltammetry reduction. Different characterization techniques such as FT-IR, HR-SEM, XRD and Raman spectroscopy were used to characterize the GO and ERGO–metalNPs. Parameters that influence the electroanalytical response of the ERGO–SbNPs and ERGO–AuNPs such as, pH, deposition time, deposition potential, purging time were investigated and optimized. Well-defined, reproducible peaks with detection limits of 0.0125 μM and 0.062 μM were obtained for BPA using ERGO–SbNPs and ERGO–AuNPs respectively. The rGO-metalNPs–PGE was used for the quantification of BPA in tap water sample and proved to be suitable for the detection of BPA below USEPA prescribed drinking water standards of 0.087 μM.

>Magister Scientiae - MSc / This project focuses on the development of simple, highly sensitive, accurate, and low cost electrochemical sensors based on the modification of pencil graphite electrodes by the electrochemical reduction of graphene oxide-metal salts as nanocomposites (ERGO-MC-PGE; MC = Sb or Au nanocomposite). The electrochemical sensors ERGO-Sb-PGE and ERGO-Au-PGE were used in the determination of paracetamol (PC) in pharmaceutical formulations using adsorptive stripping differential pulse voltammetry. The GO was prepared from graphite via a modified Hummers’ method and characterized by FTIR and Raman spectroscopy to confirm the presence of oxygen functional groups in the conjugated carbon-based structure whilst, changes in crystalline structure was observed after XRD analysis of graphite and GO. / 2023-10-07

>Magister Scientiae - MSc / This work reports the use of a pencil graphite electrode (PGE) as inexpensive and sensitive electrochemical sensing platform fabricated by using electrochemically reduced graphene oxide (ERGO) in conjunction with an in-situ plated thin mercury film. For the first time the ERGOHgF-PGE sensor is proposed for simultaneous detection of cadmium (Cd2+), copper (Cu2+), lead (Pb2+) and zinc (Zn2+) using N-Nitroso-N-phenylhydroxylamine (cupferron) as complexing agent by square-wave adsorptive cathodic stripping voltammetry (SW-AdCSV). The technique is based on the adsorption of cupferron- metal ion complexes onto the surface of the ERGO-HgFPGE at 0.1 V for 60 s carried out in 0.1 M acetate buffer solution (pH 4.6). The synthesized graphene oxide (GO) and graphene nanosheets (GNs) were characterized using different analytical techniques such as FT-IR which confirms the presence of oxygen moieties embedded in the graphitic structure and further demonstrated by UV-Vis, validating the synthesis of GO / 2023

Compared to other instruments for chemical analyses, electrochemical analyzers are relatively simple, inexpensive, easy to miniaturize and require little-to-no maintenance. However, like all commercially available instruments, commercial electrochemical analyzers like potentiostats primarily operate as black boxes with manufacturers providing little or no information about internal circuitry and programming. This practice can limit a researcher’s ability to develop new techniques or adapt an instrument for applications outside its typical use. In contrast, creators of open-source instruments release all the necessary information for reproduction of the hardware and software – minimizing such barriers to innovation in chemical analyses. Here, we report a low-cost, compact potentiostat based on an open-source Arduino microcontroller capable of performing electrochemical analyses such as cyclic and linear sweep voltammetry with an operating range of ± 208 𝜇A and ± 2.5 V. Performance of the potentiostat is investigated with low-cost pencil graphite electrodes and compared to a commercial potentiostat.

Electrochemical measurements are utilized in various fields, including healthcare (e.g., potentiometric measurements for electrolytes in blood and blood gas, amperometric biosensing of glucose as in blood glucose meters), water quality (e.g., pH measurement, voltammetric analyses for heavy metals), and energy. Much of the appeal of electrochemical analyses can be attributed to the relative simplicity, low cost and lack of maintenance associated with electrochemical instruments, along with techniques that can exhibit high sensitivity and selectivity, wide linear dynamic range, and low limits of detection for many analytes. While commercial electrochemical analyzers are less expensive than many other instruments for chemical analyses and are available from various manufacturers, versatility and performance often coincide with added expense. Recently, the development of low-cost, adaptable, open-source chemical instruments, including electrochemical analyzers, has emerged as a topic of great interest in the scientific community. In contrast to commercial instruments, for which schematics and underlying operation details are often obscured – severely limiting modifications and improvements, creators of open-source instruments release all the necessary information for reproduction of the hardware and software. As a result, open-source instruments not only serve as excellent teaching tools for novices to gain experience in electronics and programming, but also present opportunity to design and develop low-cost, portable instruments, which have particular significance for point-of-care sensing applications, use in resource-limited settings, and the rapidly developing field of on-body sensors. In this work, we report the design of a low-cost, compact electrochemical analyzer based on an open-source Arduino microcontroller. The instrument is capable of performing electrochemical analyses such as cyclic and linear sweep voltammetry with an operating range of ± 138 ��A and ± 1.65 V. Performance of the platform is investigated with low-cost pencil graphite electrodes and results compared to commercial potentiostats.

Neste trabalho foram estudadas as potencialidades eletroanalíticas de um material híbrido condutor baseado em acetato de celulose e grafite com eletrodeposição de filme condutor de Azul da Prússia (CA/G/PB) como sensor para espécies com importância biológica. O material híbrido foi preparado pelo processo de inversão de fase e caracterizado pelas técnicas de microscopia eletrônica de varredura acoplada com espectroscopia de energia dispersiva (SEM-EDS) e voltametria cíclica. O composto Azul da Prússia (PB) foi imobilizado na superfície do material por eletropolimerização, aplicando-se um potencial fixo de 20 mV em uma janela de -0,3 V a 1,2 V. Os estudos eletroquímicos do eletrodo modificado CA/G/PB foram realizados em solução de KCl 0,1 mol.L-1, sendo obtidos dois pares redox para a espécie eletroativa imobilizada com potenciais médios (E0) em 0,204 V e 0,842 V, indicando um comportamento quase-reversível. O eletrodo demonstrou alta estabilidade após 500 ciclos redox, não sendo observada lixiviação da espécie eletroativa da superfície da matriz modificada. Os dois pares redox do material híbrido CA/G/PB permaneceram praticamente constantes entre os pH 5,0 e 8,0, indicando que as intensidades de pico não são significativamente afetadas nessa faixa de pH. A correlação linear entre as intensidades de pico e a raiz quadrada da velocidade de varredura, indicou que o sistema possui um comportamento similar aqueles em que o processo é controlado por difusão das espécies eletroativas à superfície do eletrodo. O azul da Prússia imobilizado foi aplicado na determinação de dopamina (DP), ácido úrico (AU), ácido ascórbico (AA) e Paracetamol (PCT) através da técnica de voltametria cíclica, voltametria de pulso diferencial e cronoamperometria. / In this work, we studied the electroanalytical potential of a conductive hybrid material based on cellulose acetate and graphite with electrodeposition Blue conductor film of Prussia (CA / G / PB) as a sensor for species with biological importance. The hybrid material was prepared by phase inversion process and characterized by the techniques of scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS) and cyclic voltammetry. The dye of Prussian blue (PB) was immobilized on the surface of the material by electropolymerization applying a fixed potential of 20 mV in a interval from -0.3 V to 1.2 V. The electrochemical behavior of the modified electrode CA / G / PB were performed in solution of 0.1 mol L-1 KCl being obtained two redox couples for the electroactive species immobilized with midpoint potentials (E0) in 0.204 V and 0.842 V, indicating a quasi-reversible behavior. The electrode showed high stability after 500 redox cycles with no observed leaching of electroactive species to the surface of the modified electrode. The two redox pair of the CA / G / PB electrode was kept practically constant within pH 5.0 and 8.0, indicating that the peak intensities are not significantly affected in this pH range. The linear correlation between peak intensities and the square root of scan rate, indicated that the system has a similar behavior those in which the process is controlled by diffusion of electroactive species to the electrode surface. The immobilized Prussian blue was applied to determine dopamine (DP), uric acid (UA), ascorbic acid (AA) and paracetamol (PCT) by analytical techniques of cyclic voltammetry, differential pulse voltammetry and chronoamperometry.

Neste trabalho foram estudadas as potencialidades eletroanalíticas de um material híbrido condutor baseado em acetato de celulose e grafite com eletrodeposição de filme condutor de Azul da Prússia (CA/G/PB) como sensor para espécies com importância biológica. O material híbrido foi preparado pelo processo de inversão de fase e caracterizado pelas técnicas de microscopia eletrônica de varredura acoplada com espectroscopia de energia dispersiva (SEM-EDS) e voltametria cíclica. O composto Azul da Prússia (PB) foi imobilizado na superfície do material por eletropolimerização, aplicando-se um potencial fixo de 20 mV em uma janela de -0,3 V a 1,2 V. Os estudos eletroquímicos do eletrodo modificado CA/G/PB foram realizados em solução de KCl 0,1 mol.L-1, sendo obtidos dois pares redox para a espécie eletroativa imobilizada com potenciais médios (E0) em 0,204 V e 0,842 V, indicando um comportamento quase-reversível. O eletrodo demonstrou alta estabilidade após 500 ciclos redox, não sendo observada lixiviação da espécie eletroativa da superfície da matriz modificada. Os dois pares redox do material híbrido CA/G/PB permaneceram praticamente constantes entre os pH 5,0 e 8,0, indicando que as intensidades de pico não são significativamente afetadas nessa faixa de pH. A correlação linear entre as intensidades de pico e a raiz quadrada da velocidade de varredura, indicou que o sistema possui um comportamento similar aqueles em que o processo é controlado por difusão das espécies eletroativas à superfície do eletrodo. O azul da Prússia imobilizado foi aplicado na determinação de dopamina (DP), ácido úrico (AU), ácido ascórbico (AA) e Paracetamol (PCT) através da técnica de voltametria cíclica, voltametria de pulso diferencial e cronoamperometria. / In this work, we studied the electroanalytical potential of a conductive hybrid material based on cellulose acetate and graphite with electrodeposition Blue conductor film of Prussia (CA / G / PB) as a sensor for species with biological importance. The hybrid material was prepared by phase inversion process and characterized by the techniques of scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS) and cyclic voltammetry. The dye of Prussian blue (PB) was immobilized on the surface of the material by electropolymerization applying a fixed potential of 20 mV in a interval from -0.3 V to 1.2 V. The electrochemical behavior of the modified electrode CA / G / PB were performed in solution of 0.1 mol L-1 KCl being obtained two redox couples for the electroactive species immobilized with midpoint potentials (E0) in 0.204 V and 0.842 V, indicating a quasi-reversible behavior. The electrode showed high stability after 500 redox cycles with no observed leaching of electroactive species to the surface of the modified electrode. The two redox pair of the CA / G / PB electrode was kept practically constant within pH 5.0 and 8.0, indicating that the peak intensities are not significantly affected in this pH range. The linear correlation between peak intensities and the square root of scan rate, indicated that the system has a similar behavior those in which the process is controlled by diffusion of electroactive species to the electrode surface. The immobilized Prussian blue was applied to determine dopamine (DP), uric acid (UA), ascorbic acid (AA) and paracetamol (PCT) by analytical techniques of cyclic voltammetry, differential pulse voltammetry and chronoamperometry.

Neste trabalho foram estudadas as potencialidades eletroanalíticas de um material híbrido condutor baseado em acetato de celulose e grafite com eletrodeposição de filme condutor de Azul da Prússia (CA/G/PB) como sensor para espécies com importância biológica. O material híbrido foi preparado pelo processo de inversão de fase e caracterizado pelas técnicas de microscopia eletrônica de varredura acoplada com espectroscopia de energia dispersiva (SEM-EDS) e voltametria cíclica. O composto Azul da Prússia (PB) foi imobilizado na superfície do material por eletropolimerização, aplicando-se um potencial fixo de 20 mV em uma janela de -0,3 V a 1,2 V. Os estudos eletroquímicos do eletrodo modificado CA/G/PB foram realizados em solução de KCl 0,1 mol.L-1, sendo obtidos dois pares redox para a espécie eletroativa imobilizada com potenciais médios (E0) em 0,204 V e 0,842 V, indicando um comportamento quase-reversível. O eletrodo demonstrou alta estabilidade após 500 ciclos redox, não sendo observada lixiviação da espécie eletroativa da superfície da matriz modificada. Os dois pares redox do material híbrido CA/G/PB permaneceram praticamente constantes entre os pH 5,0 e 8,0, indicando que as intensidades de pico não são significativamente afetadas nessa faixa de pH. A correlação linear entre as intensidades de pico e a raiz quadrada da velocidade de varredura, indicou que o sistema possui um comportamento similar aqueles em que o processo é controlado por difusão das espécies eletroativas à superfície do eletrodo. O azul da Prússia imobilizado foi aplicado na determinação de dopamina (DP), ácido úrico (AU), ácido ascórbico (AA) e Paracetamol (PCT) através da técnica de voltametria cíclica, voltametria de pulso diferencial e cronoamperometria. / In this work, we studied the electroanalytical potential of a conductive hybrid material based on cellulose acetate and graphite with electrodeposition Blue conductor film of Prussia (CA / G / PB) as a sensor for species with biological importance. The hybrid material was prepared by phase inversion process and characterized by the techniques of scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS) and cyclic voltammetry. The dye of Prussian blue (PB) was immobilized on the surface of the material by electropolymerization applying a fixed potential of 20 mV in a interval from -0.3 V to 1.2 V. The electrochemical behavior of the modified electrode CA / G / PB were performed in solution of 0.1 mol L-1 KCl being obtained two redox couples for the electroactive species immobilized with midpoint potentials (E0) in 0.204 V and 0.842 V, indicating a quasi-reversible behavior. The electrode showed high stability after 500 redox cycles with no observed leaching of electroactive species to the surface of the modified electrode. The two redox pair of the CA / G / PB electrode was kept practically constant within pH 5.0 and 8.0, indicating that the peak intensities are not significantly affected in this pH range. The linear correlation between peak intensities and the square root of scan rate, indicated that the system has a similar behavior those in which the process is controlled by diffusion of electroactive species to the electrode surface. The immobilized Prussian blue was applied to determine dopamine (DP), uric acid (UA), ascorbic acid (AA) and paracetamol (PCT) by analytical techniques of cyclic voltammetry, differential pulse voltammetry and chronoamperometry.

Differential pulse voltammetry (DPV) was used for developing a method for the determination of phenothiazine derivatives, namely chlorpromazine (CHP) and levomepromazine (LMP), using a glassy carbon electrode (GCE) and a graphite electrode, both with a 2 mm disc diameter. Comparison of quantification limits (LQ) for both substances on both electrodes was performed. After optimizing and processing the results, the optimal conditions for measuring calibrations were as follows: Britton- Robinson (BR) buffer at pH 4.0. Calibration dependences were measured inthe concentration range from 1·10-7 to 1·10-4 mol·dm-3 . There was no need for electrochemical electrode regeneration or matrix pretreatment. The results showed higher measurement sensitivity for CHP, and the graphite electrode also showed higher sensitivity. Although there were measured lower concentrations with the graphite electrode in comparison to the GCE, because of the low repeatability of the measurements in the lower concentration range 1-10·10-7 mol·dm-3 , the LQ is comparable to the results reached on the GCE. Besides to the BR buffer, measurements in other matrices (drinking water and river water) were also made. The following LQ values were achieved: 1.0·10-6 mol·dm-3 (in BR buffer), 1.1·10-6 -1.4·10-6 mol·dm-3 (in drinking water) and...