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This thesis contains two major sections. The first section is dealing with the preparation of conductive polymers-based sorbents while the second section is mostly focused on the synthesizing nanocomposites by electrospinning. All the prepared sorbents and nanofibers have been utilized to isolate some organic compounds in environmental and biological samples. Section I:In the first chapter, an unbreakable solid phase microextraction fiber coating based on aniline-silica nanocomposite was electrodeposited on a stainless steel wire. The electropolymerization process was carried out at a constant deposition potential, applied to the corresponding aqueous electrolyte containing aniline and...