Real-time monitoring of photoinduced atom transfer radical polymerization by time-resolved diffusion NMR

Abstract

Conventional real-time monitoring of polymerization is a laborious process that requires offline sampling and analysis. In this work, we introduce an advanced approach that combines Time-Resolved Diffusion NMR with ¹H NMR for the simultaneous, in situ tracking of both monomer conversion and molecular weight evolution. We successfully applied this method to monitor the photoinduced atom transfer radical polymerization (photo-ATRP) in real-time. Furthermore, by coupling the gamma model with dispersity-matched accumulation, we accurately determined the dispersity values of the resulting polymers. To make the method more accessible, we developed a user-friendly program that sets up the acquisition and simplifies real-time monitoring of photo-ATRP. Additionally, the program allows stopping illumination at any desired monomer conversion, enabling easy control of the process.