Abstract

European Journal of Mass Spectrometry
Volume 15 Issue 2, Pages 231–238 (2009)
doi: 10.1255/ejms.946

Preliminary silylation for structure determination of oligomeric silsesquioxanes by matrix-assisted laser desorption/ionisation mass spectrometry

V.G. Zaikin,^a,* R.S. Borisov,^a N.Yu. Polovkov,^a S.N. Filatov^b and V.V. Kireev^b
aTopchiev Institute of Petrochemical Synthesis, Russian Academy of Sciences, Leninsky prospect 29, 119991 Moscow, Russia. E-mail: zaikin@ips.ac.ru
^bPolymer Chemistry and Technology Department, D. Mendeleev University of Chemical Technology of Russia, Moscow, Russia

The potential of preliminary silylation for the determination of numbers of hydroxyl groups in separate molecules of oligomeric silsesquioxanes by matrix-assisted laser desorption/ionisation mass spectrometry has been demonstrated for the first time. Derivatisations allowing the introduction of trimethylsilyl, tert-butyldimethylsilyl and pentafluorophenyldimethylsilyl groups were tested. It was shown that more reliable structure elucidation of individual oligomers can be achieved knowing the number of hydroxyl groups thus determined.

Keywords: silylation, silsesquioxanes, mass spectrometry, matrix-assisted laser desorption/ionisation

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