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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. Filatovb and V.V. Kireevb
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
ABSTRACT:
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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