Introduction of Air-Segmentation Approach to Flow Titration by Feedback-based and Subsequent Fixed Triangular Wave-controlled Flow Ratiometry

Abstract

An air-segmentation approach has been introduced to a feedback-based and subsequent fixed triangular wave-controlled flow ratiometry to suppress axial dispersion in flow titration. The flow rate of a base solution containing an indicator is linearly varied with a control signal, V_c, supplied by a computer. The solution is merged with an acid solution under a constant total flow rate. Air is introduced to the merged solution in order to segment the solution with air bubbles. Both phases are led to a UV/Vis detector without phase separation. Air signals are removed by signal processing. The effect of the lag time between the merging of solutions upstream and the sensing of the corresponding signal downstream is offset by feedback-based upward and downward V_c scans, and thus the V_c that gives the equivalence composition is determined. Subsequently, fixed triangular wave control is applied to a narrower V_c range with a higher scan rate to enhance the throughput rate (maximally 11.8 titrations/min). Air-segmentation has been found to be effective to reduce axial dispersion and to preserve the titrand/titrant composition upon their just being merged. Consequently, the applicable range is extended especially to lower titrand concentration. The proposed method has been successfully applied to various acid-base titrations, including the nonaqueous titration of the Japanese Pharmacopoeia drug.