Characterization of silsesquioxanes by size-exclusion chromatography and matrix-assisted laser desorption/ionization time-of-flight mass spectrometry

Liquid chromatography in combination with spectroscopic methods like matrix‐assisted laser desorption/ionization time‐of‐flight mass spectrometry (MALDI‐TOFMS) or nuclear magnetic resonance (NMR) spectroscopy is a powerful method to characterize silsesquioxanes and silsesquioxane mixtures. As new examples, the formation of silsesquioxyl‐substituted silsesquioxanes [(n‐octyl)7(SiO1.5)8]2O and [(n‐octyl)7(SiO1.5)8O]2[(n‐octyl)6(SiO1.5)8] as well as the cage rearrangement of octa‐[(n‐heptyl)silsesquioxane] to larger structur es [(n‐heptyl)SiO1.5)]n up to n=28 are shown. Copyright © 2003 John Wiley & Sons, Ltd.