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Characterization of a [(O 3/2 SiMe) x (OSi(OH)Me) y (OSiMe 2 ) z ] silsesquioxane copolymer resin by mass spectrometry
Author(s) -
Tecklenburg Ron E.,
Wallace William E.,
Chen Huiping
Publication year - 2001
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.494
Subject(s) - chemistry , mass spectrometry , fourier transform ion cyclotron resonance , silsesquioxane , oligomer , electrospray ionization , sample preparation in mass spectrometry , dispersity , monomer , mass spectrum , analytical chemistry (journal) , gel permeation chromatography , time of flight mass spectrometry , chromatography , polymer chemistry , ionization , ion , organic chemistry , polymer
Abstract Electrospray ionization Fourier transform ion cyclotron resonance (ESI‐FTICR) mass spectrometry and matrix‐assisted laser desorption/ionization time‐of‐flight (MALDI‐TOF) mass spectrometry were applied to a complex silsesquioxane‐siloxane copolymer resin. The wide‐polydispersity starting material was fractionated into 21 separate fractions in order to facilitate the analysis by mass spectrometry. ESI‐FTICR exact mass measurements were able to identify the specific oligomers present in the lowest mass fractions and showed that very few unreacted silanol groups remained, that is, topologically closed structures predominated. MALDI‐TOFMS was able to show that gel‐permeation chromatography substantially underestimated the molecular masses of the higher mass fractions. Mass autocorrelation was able to show that the silsesquioxane monomer appeared only in even numbers in any given oligomer. This is a natural consequence of the highly condensed nature of the resin. Copyright © 2001 John Wiley & Sons, Ltd.