Ion-exclusion chromatography (ICE) followed by ion chromatography (IC) was
used for the determination of trace anionic contaminants in concentrated we
ak acids. The ICE separation was used as a pretreatment step to isolate the
contaminant anions of strong acids 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 addr
ess the increased purity requirements for use of these concentrated acids i
n semiconductor applications. The chromatographic conditions were optimized
for determining trace chloride, sulfate, phosphate, and nitrate in concent
rated 24.5% (v/v) hydrofluoric acid; trace chloride, sulfate, and nitrate i
n concentrated 85% (w/w) phosphoric acid and trace chloride and sulfate in
concentrated 0.7% (v/v) glycolic acid. Method detection Limits for the anio
ns of interest were below 100 mu g/l. (C) 1999 Elsevier Science B.V. All ri
ghts reserved.