title: Structural characterization of telechelic polyisobutylene diol.
abstract: 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.
authors.affiliation: Polymer Science Program, Department of Chemistry, University of Massachusetts Lowell, One University Avenue, Lowell, Massachusetts 01854, USA.
authors.forename: Sanjib
authors.initials: S
authors.lastname: Banerjee
authors.affiliation: Polymer Science Program, Department of Chemistry, University of Massachusetts Lowell, One University Avenue, Lowell, Massachusetts 01854, USA.
authors.forename: Priyank N
authors.initials: PN
authors.lastname: Shah
authors.affiliation: Division of Advanced Materials Science and Department of Chemistry, Pohang University of Science and Technology (POSTECH), Pohang, Pohang 790-784, South Korea.
authors.forename: Youncheol
authors.initials: Y
authors.lastname: Jeong
authors.affiliation: Division of Advanced Materials Science and Department of Chemistry, Pohang University of Science and Technology (POSTECH), Pohang, Pohang 790-784, South Korea.
authors.forename: Taihyun
authors.initials: T
authors.lastname: Chang
authors.affiliation: Boston Scientific Corporation, 4100 Hamline Ave. North, St. Paul, Minnesota, 55112, USA.
authors.forename: Kasyap
authors.initials: K
authors.lastname: Seethamraju
authors.affiliation: Polymer Science Program, Department of Chemistry, University of Massachusetts Lowell, One University Avenue, Lowell, Massachusetts 01854, USA. Electronic address: Rudolf_Faust@uml.edu.
authors.forename: Rudolf
authors.initials: R
authors.lastname: Faust
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods; D011108:Polymers / Q000737:chemistry*; D019032:Spectrometry, Mass, Matrix-Assisted Laser Desorption-Ionization / Q000379:methods
chemical_list: D011108:Polymers
keywords: Chemical homogeneity; Gradient HPLC; Liquid chromatography at critical conditions; Living cationic polymerization; Matrix-assisted laser desorption/ionization time-of-flight mass spectrometry; Polyisobutylene diol