A bismuth-coated carbon fiber microelectrode was prepared using cyclic voltammetry (CV). An analytical application was performed for the copper analysis with Square Wave Stripping Voltammetry (SWSV). Gallic acid n-propyl ester (PG) was used for the complex formation with a copper ion, and electrochemical measurements were performed with a pre-amplifier of a low-current module for nano amper detection. The effects of various parameters on the response were optimized. Analytical working ranges of 0.03-25.9 μgl-1 and 0-25 mgl-1 Cu(II) were obtained. The relative standard deviation at 13 mgl-1 Cu was 0.9% (n = 12) in optimum conditions. The detection limit was found to have been 0.019 μgl-1, with a 30-sec accumulation time. The developed methods were applied to a copper assay in water samples.