With the aid of atomic absorption, a systematical and analytical evaluation method called Taguchi's quality engineering has been applied for the separation of copper ions from a solution using a laboratory electrodialysis set-up to evaluate the optimal experimental conditions and hence to achieve the highest removal percentage and the best robustness of the quantitation from the least number of experimental runs. Four parameters at three levels were studied: concentration (100, 500, 1000 ppm), temperature (25, 40, 60 degreesC), flow rate (0.07, 0.7, 1.2 mL/s) and voltage (10, 20, 30 V). Two types of different membranes with different ion-exchange capacities were used. The optimal levels thus determined for the four influential factors were: concentration 1000 ppm, temperature 60 degreesC, flow rate 0.07 mL/s and voltage 30 V. It has also been found that using a membrane pair with higher ion-exchange capacity improves performance. The highest removal percentage was found to be 94.94% and 97.33% for the two types of membranes.