A novel fiber optic mid-IR probe equipped with an Attenuated Total Reflecta
nce (ATR) head and a transmission (TR) head was developed for the real-time
monitoring of polymerization processes. The TR head can monitor very low c
oncentrations (0.1 mmol/L), The probe was used to monitor both homogeneous
(living) and heterogeneous (slurry) isobutylene (IB) polymerizations by fol
lowing the disappearance of IR bands characteristic of is, and the appearan
ce of IR bands characteristic polyisobutylene (PIB), Due to the sensitivity
of the TR probe is consumption could also be followed by monitoring an ove
rtone signal. In the case of the living polymerization initiated by a novel
substituted epoxide the TR probe gave insight into the initiation reaction
as well.