Abstract: The 3-mercaptopropylsulfonic acid (MPSA) breakdown product of the bis(sodiumsulfopropyl)disulfide (SPS) additive used in acid copper plating baths accelerates copper electrodeposition and can be detected by cyclic voltammetric stripping (CVS) analysis. In the presence of oxygen, MPSA decomposes rapidly in acid copper sulfate baths so that the CVS stripping peak area (Ar) decreases on successive cycles. The slope of a plot of Ar vs. CVS cycle number (or time) or logarithm of the CVS cycle number (or time) provides a measure of the initial MPSA concentration.

Abstract: The concentration of citrate complexing agent in an electroless cobalt or nickel plating bath is determined by titrating a sample of the electroless plating bath containing a small concentration of free fluoride ion with a standard lanthanum nitrate solution. During the titration, La3+ ion first reacts preferentially with the citrate complexing agent and then with fluoride ion, which reduces the free fluoride ion concentration. The endpoint for the titration is indicated by a substantial decrease in the free fluoride ion concentration, which is detected via a fluoride ion specific electrode (ISE). The method can be used for analysis of other complexing agents.

Abstract: The concentration of citrate complexing agent in an electroless cobalt or nickel plating bath is determined by titrating a sample of the electroless plating bath containing a small concentration of free fluoride ion with a standard lanthanum nitrate solution. During the titration, La3+ ion first reacts preferentially with the citrate complexing agent and then with fluoride ion, which reduces the free fluoride ion concentration. The endpoint for the titration is indicated by a substantial decrease in the free fluoride ion concentration, which is detected via a fluoride ion specific electrode (ISE). The method can be used for analysis of other complexing agents.

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.