Improved Voltammetric Procedure for Chloride Determination in Highly Acidic Media

Area of Science:

• Electrochemistry
• Analytical Chemistry

Background:

• Chloride ions are crucial in copper electroplating baths.
• Direct determination of chloride ions via oxidation is unreliable due to interfering species.
• Existing methods may require sample pretreatment or lack speed.

Purpose of the Study:

• To develop an optimized cyclic voltammetry method for accurate chloride ion determination.
• To establish a reliable quantification method for chloride in acid copper electroplating baths.
• To create a fast, reagent-free analytical technique for electroplating bath monitoring.

Main Methods:

• Cyclic voltammetry (CV) was employed to analyze chloride ions.
• Experimental parameters were optimized using statistical tools.
• A calibration curve was established based on the reduction current of generated chlorine gas.

Main Results:

• The optimized CV method reliably determines chloride ions from 10 to 200 mg/dm³.
• A linear relationship was observed between chloride concentration and the voltammetric reduction current.
• The analysis time per sample is under 20 minutes.

Conclusions:

• The developed cyclic voltammetry method provides a fast, accurate, and direct quantification of chloride ions in copper electroplating baths.
• This technique eliminates the need for sample pretreatment and additional reagents.
• The method is suitable for automated, high-throughput analysis in industrial settings.