For the past three decades, Cyclic Voltammetric Stripping (CVS) has been the standard practice for analyzing organic additives in electroplating copper baths in the circuit board and wafer plating industries. The variations in the compositions of such baths have created a need for more optimized method development routines. New advancements in the hardware and software protocols for CVS have simplified the overall process of method optimization to a great extent. In this study, the process of method optimization is discussed in conjunction with these protocols.