Analytical chemistry offers useful tools to solve problems in industrial laboratories caused by traditional methods of analysis. A simple ion chromatographic method has been developed to determine chloride, bromide, nitrate, and sulfate in hexafluorosilicic acid and tetrafluoroboric acid. These materials contain high levels of fluorinated species at pH values lower than 1.0, which represent a challenging sample. Currently, these matrixes are analyzed by chemical methods with associated interferences. Optimization of the ion chromatography method was performed using industrial samples due to the absence of reference materials. In order to obtain the best chromatographic resolution, the sample dilution, flow rate, and eluent concentration were studied in an isocratic mode. The method was suitable for the separation of the anions in less than 30 minutes, without sample treatment other than dilution. Good linearity was obtained with correlation coefficients between 0.9951 and 0.9998. Limits of quantification were between 0.21 and 0.39 mg/L for chloride, bromide, nitrate, and sulfate in hexafluorosilicic acid and tetrafluoroboric acid, and the inter- and intra-day relative standard deviations were less than 15%.