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Abstract Electrochemistry has many features making it a unique technique for choice when analyzing real sample. Electrochemical techniques have the advantages of low cost, instrumental simplicity and portability in addition to high sensitivity and selectivity as well as wide linear range with low detection limits. This makes electroanalytical techniques among the most favorable analytical methods for different applications. In particular, voltammetric sensors are an important category of electrochemical sensors. This thesis describes the development and electrochemical characterization and analytical applications of two voltammetric sensors developed for dopamine (DA) and glucose detection. Nickel nanoparticles (Ni-NP) based sensors and nickelcopper nanoparticles (Ni/CuNPs) based sensors were developed for the selective detection of dopamine and glucose, respectively. This thesis is divided into three chapters. A brief description of each chapter is given below: Chapter I: this chapter provides a general overview for nanomaterials, classification of nanomaterials, important tools to characterize nanomaterials and applications of nanoscience in electrochemistry. In addition, this chapter includes a general introduction on various electroanalytical techniques. Moreover, this chapter describes the different types of chemical sensors and discusses in detail voltammetric sensors, and the important concepts of voltammetric methods relevant to the thesis work.Chapter II: This chapter represents the fabrication of nickel nanoparticles based sensor for the selective determination of dopamine. The composition and the electrochemical behavior of the developed nano nickel modified glassy carbon electrode (nano-Ni-nafion/GCE) and nano nickel modified graphite electrode (nano-Ninafion/ GE)were investigated by field emission scanning electron microscope (FESEM),X-ray diffraction spectroscopy (XRD),cyclic voltammetry(CV) and differential pulse voltammetry (DPV). The results indicated the formation of stable nano-Ni nafion film on the surface of glassy carbon and graphite electrodes. The developed sensor was shown to have excellent electrocatalytic activity, excellent reproducibility and stability towards the oxidation of dopamine. Different parameters affecting the analytical performance of the developed sensors were investigated, including: number of cycles, concentration of NaOH, concentration of NiSO4 and scan rate. Under optimized conditions, the response of the prepared modified electrodes towards dopamine was found to be linear in the concentration range 1-2000 Ppmwith a detection limit of 1.62 μM (nano-Ninafion/ GCE) and 0.29μM (nano-Ni-nafion/GE). DA sensors exhibited a sensitivity of 13.8, 61.3 mA L-1mol for nano-Ni-nafion/GCE and nano-Ni-nafion/GE, respectively. Chapter III: This chapter deals with the development of nickel copper nanoparticles based sensor for the glucose. The composition and the electrochemical behavior of the developed nano nickel-copper modified glassy carbon electrode (nano-Ni/Cu GCE) were investigated by field emission scanning electron microscope (EFSEM), energy dispersive X-ray spectrometer (EDX), cyclic voltammetry (CV) and differential pulse voltammetry (DPV). The results indicated the formation of high quality and stable nano Ni-Cu film on the surface of glass carbon (GC) electrode. This nano Ni-Cu sensor could effectively oxidize glucose with high catalytic activity compared to only Ni or Cu films. Different parameters affecting the analytical performance of the developed nano Ni-Cu sensor were investigated, including: copper concentration, nickel concentration and number of cycles. Under optimized conditions, the response of the prepared modified electrode towards glucose was found to be linear in the concentration range (0.25 to 30 mM) with a sensitivity of 20.78μAmol−1L) and low detection limit (30μM). The sensor was utilized for the analysis of glucose in blood serum sample and the results obtained were correlated to those observed using the commercial glucose sensor. |