Monitoring solid phase synthesis reactions with electrochemical impedance spectroscopy (EIS)

Abstract

This work describes the use of electrochemical impedance spectroscopy (EIS) as a means to monitor solid phase synthesis on resin beads. EIS was used to track changes during the swelling of beads in various solvents, during three typical reactions and throughout cleavage of the final product from the bead. The impedance response was investigated in a chemical reactor and was found to be faintly sensitive to the resin swelling and solvent flow. The position of the electrode within the reactor was found to be critical as polystyrene based beads float or sink dependent upon the solvent used. However, by choosing electrode position it was possible to monitor reaction progress on beads or within the bulk reactant/product mixture. Of the three typical chemical reactions studied impedance spectroscopy successfully followed two. Fitting of the impedance data to an equivalent electrical circuit provided an estimate as to the relative contribution of capacitive and resistive components to the overall response. Kinetic data from two reactions were also modelled, in both cases complex kinetics was observed, in close agreement with other studies.