Structural characterization of telechelic polyisobutylene diol

The chemical homogeneity of telechelic polyisobutylene diol (PIB-diol), prepared by hydroboration-oxidation of allyl telechelic PIB obtained by reacting living PIB with allyltrimethylsilane, was investigated by liquid chromatography at critical conditions (LCCC) and HPLC coupled with matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS). A normal phase gradient HPLC method was developed that was able to separate the as-synthesized PIB-diol into three components; PIB-diol, PIB-monool and PIB without any OH functionality. These were analyzed by MALDI-TOF MS, which suggested that the reaction of living PIB with allyltrimethylsilane was incomplete. LCCC using refractive index (RI) detector as a concentration detector allowed separation and quantification of PIB species according to their chemical heterogeneity (PIB-diol = 95.3%, PIB-monool = 3.3%, non-functional PIB = 1.4%). The calculated number average functionality (Fn) of PIB-diol = 1.94 suggests high quality of PIB-diol suitable for high molecular weight polyurethane synthesis.