Abstract: The concentration of chloride ion in an acid copper electroplating bath is determined from the effect that chloride exerts on the copper electrodeposition rate in the presence of organic additives. A cyclic voltammetric stripping (CVS) rate parameter is measured, before and after standard addition of a plating bath sample, in an acid copper electrodeposition solution containing little or no chloride and at least one organic additive. Cross contamination and waste disposal issues associated with the reagents and reaction products involved in chloride titration analyses are avoided. The method may also be applied to analysis of other halides (bromide and iodide) and other solutions.