In this study, electrochemically reduced graphene oxide (ERGO) was used for the preparation of a screen‐printed modified electrode and applied for the voltammetric determination of fenamiphos (FNP) in tomato samples. Graphene oxide (GO) used for sensor construction was prepared according to an improved Hummers method and characterized by XRD, TEM, and FTIR, which confirmed the nanomaterial obtention. The ERGO formation was carried out from the electrodeposition by cyclic voltammetry, at 50 mV s−1 in the potential range of 0.0 to −1.5 V, during 50 cycles. ERGO‐SPE was used in the evaluation of the voltammetric behavior of FNP. The ERGO‐SPE proposed presented excellent electrochemical performance towards FNP oxidation, promoting an enhance on the anodic peak current and a decrease of peak potential. Under optimized conditions, it was possible to construct an analytical curve, using square wave voltammetry, with a linear region of 0.25 to 25.0 μM, with calculated limits of detection and quantification of 0.067 and 0.22 μM. From this, it was possible to analyze FNP in fortified tomato samples at three concentration levels, which showed recoveries values varying between 82 and 102 %. The ERGO‐SPE device proved useful in determining FNP, where the effect of the electrodeposition of the GO promoted a significant increase in the employability of the printed electrode.
Resumo: O presente manuscrito descreve o desenvolvimento de um sensor descartável sensível e seletivo baseado em filmes de polipirrol dopados (PPy) para determinação íons fluoreto. Os íons fluoretos foram incorporados na matriz PPy durante a polimerização eletroquímica realizada em condições galvanostáticas em um eletrodo compósito etileno vinil acetato e negro de fumo. Parâmetros experimentais envolvidos na preparação de película PPy tais como densidade de corrente elétrica, carga elétrica, o pH e a concentração de eletrólito foram otimizados de forma a maximizar a resposta potenciométrica. A resposta do sensor para íons de flúor foi linear no intervalo de concentração de 1,00 × 10 -5 a 1,08 × 10 -2 mol L -1, com uma inclinação de ~ 40 mV / pF e foi estável suficiente para várias determinações. O método foi aplicado com sucesso na determinação de íons fluoreto em amostras comerciais farmacêuticas. Os resultados demonstraram que o sensor proposto pode ser utilizado como uma alternativa interessante aos métodos analíticos tradicionais para determinação de íons fluoreto.
Palavras-chave: Filmes de polipirrol, íons fluoreto, eletrodos íon-seletivo, eletrodo compósito.
Polypyrrole Films Applied to Development of Disposable Ion-selective Electrode for Fluoride Ions DeterminationAbstract: This manuscript describes the development of a sensitive and selective disposable potentiometric sensor based on doped polypyrrole films (PPy) for fluoride ions determination. The fluoride ions were incorporated in the PPy matrix during electrochemical polymerization under galvanostatic conditions on a composite electrode of ethylene vinyl acetate and black carbon. Experimental parameters involved in PPy film preparation, such as electric current densities, electric charge, pH and electrolyte concentration, were optimized in order to maximize the potentiometric response. The sensor response for fluoride ions was linear in the concentration range of 1.00 × 10 -5 to 1.08 × 10 -2 mol L -1 , with a slope of ~40 mV/pF, and it was sufficiently stable for several determinations. The method was successfully applied in the determination of fluoride ions in pharmaceutical commercial samples. Results demonstrated that the proposed sensor can be used as an interesting alternative to traditional analytical methods for fluoride ions.
Keywords: Polypyrrole films, fluoride ions, ions-selective electrode, composite electrode.
IntroduçãoO desenvolvimento de sensores eletroquímicos vem sendo amplamente explorado nos últimos anos, devido a características apresentadas por estes dispositivos tais como: baixos limites de detecção, alta seletividade e estabilidade [1] . Dentre as diversas possibilidades de resposta dos sensores eletroquímicos, podemos destacar os potenciométricos devido à simplicidade operacional e o baixo custo. Destaque para os eletrodos íon-seletivo (ISE) de membrana que permitem a determinação dos mais diversos analitos com alta seletividade, baixos limites de detecção e poucos efeitos de interferência da matriz [2] . O uso de polímeros...
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