Comparison of two Cryptand separator columns for the determination of trace chloride in semiconductor-grade nitric acid

Improved ion-chromatographic approaches for measuring trace chloride in nitric acid are presented. Two columns, the IonPac Cryptand A1 and a higher-capacity Cryptand prototype, were tested and compared. Also, the use of a Continuously Regenerated Anion Trap Column (CR-ATC) was evaluated for its ability to purify electrolytically generated eluent. Nitric acid (70%) was used as the test matrix and chloride was used as the test analyte; prior to injection, the nitric acid was diluted to 0.7% for the A1 column and to 2.8% for the prototype column. Chloride could be quantified in only 20 min on either column; detection limits computed for 70% HNO3 (at 95% confidence, α = β = 2.5%) were 1.8 and 1.5 ppm for the A1 and prototype columns, respectively. Results also showed that the CR-ATC was necessary for obtaining acceptable acid blanks.