Abstract: The behavior of absorption spectroelectrochemistry of copper and the effects of instrumental equipment as well as measurement conditions on the sensitivity of copper were investigated. Results show that the best sensitivity (0.029ppm) was obtained when the electrolytic cell with double electrodes and hollow cathode light source in place of the electrolytic cell with single work electrode and deuterium lamp was used for measurement of absorption spectroelectrochemistry of copper. The technique yields increased in sensitivity of copper of 2.5-fold, in comparison to the west method.