An automated polymer synthesis platform based on an inline low-field nuclear magnetic resonance spectrometer is developed. Flow chemistry and automated inline analyses are an excellent combination for automated kinetic screening and for self-optimizing reactions with programmable conversion targeting. By monitoring monomer conversion over a continuous range of reactor residence times, the platform is able to construct kinetic profiles of polymerizations in an accurate and efficient way. The machine-assisted self-optimization routine allows the reaction to be stopped at any given preselected conversion, giving rise to unprecedented reproducibility in polymer synthesis.