An ion Chromatographic approach to the acid assay of mineral acid pickling baths of the type encountered in the stainless steel and specialty alloy industry is described. Hydrofluoric, hydrochloric, nitric, and sulfuric acids can be determined in the presence of each other and in a wide range of concentrations. An indirect approach utilizing the concentration of hydrogen ion as obtained by alkalimetry is used to correct for the presence of metal ions. The ion chromatographic technique represents a significant time advantage over wet chemical methods.