Cu(In,Ga)Se2 (CIGS) is one of the most advanced absorber materials with conversion efficiencies reaching up to about 20%. Electrodeposition of CIGS precursors is highly attractive due to its low cost, efficient utilization of raw materials and scalability to high-volume manufacturing, however, a strict chemistry control of the plating baths is required in a manufacturing environment to ensure a consistent plating process with high yields. In the present study, we tested the use of ion chromatography (IC), for the quantitative analysis of both the cationic and anionic species in a variety of aqueous alkaline electroplating solutions we developed for the fabrication of CIGS precursors. Using ion chromatography we were able to precisely determine the concentrations of several key anions commonly employed in the plating baths including chloride, sulfate, selenite, selenate, tartrate, citrate, gluconate, and ethylenediaminetetraacetate. Our results indicated IC might not be a suitable method to determine the cationic concentrations for Cu, In, Ga ions when complexing species, such as ethylenediaminetetraacetate, are present in the electroplating solutions. We determined that inductively coupled plasma optical emission spectroscopy (ICP-OES) could be used instead for the precise determination of the cationic concentrations.