Development of an Electrochemical Methodology for Analytical Monitoring of a Manganese Electrolytic Bath

Abstract Electrolytic manganese is essential for the metallurgical industry; therefore, electrolytics baths for its production have become excellent alternative, making their analytical control a priority. In this research, a carbon paste electrode (CPE) modified with bismuth powder (CPE-Bi) was developed for the first time for Mn2+ determination by square wave anodic stripping voltametric (SWASV), allowing the Mn quantification in samples from an electrolytic bath, facilitating its monitoring. A univariate method was used to optimize the CPE-Bi composition, pH, and the electrodeposition parameters, maximizing the analytical signal in Mn2+ determination through the anodic peak current (Iap). The parameters related to the square wave anodic stripping voltammetry (SWASV) were optimized by Box Behnken experimental design. The proposed methodology was successfully applied to determine Mn2+ in electrolytic bath samples, achieving recovery percentages of 96.29% ± 9.25%, suggesting it is suitable for Mn monitoring. The limit of detection of 6.5x10-6 M, sensitivity of 7.5726 μA μM-1 in a lineal range of 2.17x10-5 M to 1x10-4 M with precision of 3.27%, highlight the method’s great sensitivity, precision, and accuracy, attributed to the properties provided by bismuth powder and the electrochemical technique used, making it an excellent alternative for the Mn2+ analysis in the mining industry.