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A water sensor for a nonaqueous solvent was fabricated using poly(1,5-diaminonapthalene (DAN) nanofibers, which were prepared through a catalytic chemical polymerization of the DAN monomer using Fe(III) salt as the catalyst. Poly(1,5-DAN) nanofibers were characterized by atomic force microscope (AFM), transmission electron microscope (TEM), scanning electron microscope (SEM), and UV-vis spectroscopy. The electrochemical properties of poly(1,5-DAN) nanofibers were investigated using cyclic voltammetry (CV). The electrochemical activity of poly(1,5-DAN) nanofibers was utilized for water sensing. The fabrication of water sensor was followed by placing one drop (about 2 [micro]L) of 0.01% poly(1,5-DAN) nanofibers solution in the gap between two split gold electrodes (PBSA) and completely dried. The response of the water sensor in an acetonitrile solution was evaluated under optimized conditions. The linear dynamic range was from 0.05 to 20%, and the detection limit was determined to be 0.01%. The response of this sensor was shown to be comparable to that obtained with the Karl Fischer titration method.