Determination of trace anions in concentrated weak acids by ion chromatography.

Ion-exclusion chromatography (ICE) followed by ion chromatography (IC) was used for the determination of trace anionic contaminants in concentrated weak acids. The ICE separation was used as a pretreatment step to isolate the contaminant anions of strong acid from the excess of matrix ions. Then a fraction containing the analyte ions was separated using IC with suppressed conductivity detection. Microbore-ion-exchange columns were chosen to address the increased purity requirements for use of these concentrated acids in semiconductor applications. The chromatographic conditions were optimized for determining trace chloride, sulfate, phosphate, and nitrate in concentrated 24.5% (v/v) hydrofluoric acid; trace chloride, sulfate, and nitrate in concentrated 85% (w/w) phosphoric acid and trace chloride and sulfate in concentrated 0.7% (v/v) glycolic acid. Method detection limits for the anions of interest were below 100 micrograms/l.