UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of silsesquioxanes obtained by the hydrolytic condensation of (3-glycidoxypropyl)-trimethoxysilane in an epoxidized solvent

Silsesquioxanes obtained by the bydrolytic condensation of (3-glycidoxypropyl)trimethoxysilane (GPMS) in diglycidyl ether of bisphenol A (DGEBA) were characterized by electraspray ionization time-of-flight mass spectrometry (ESI-TOF MS) and matrix-assisted ultraviolet laser desorption/ionizatian tim...

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Autor principal: Erra Balsells, Rosa
Publicado: 2001
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Acceso en línea:https://bibliotecadigital.exactas.uba.ar/collection/paper/document/paper_10221352_v202_n11_p2425_Williams
http://hdl.handle.net/20.500.12110/paper_10221352_v202_n11_p2425_Williams
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spelling paper:paper_10221352_v202_n11_p2425_Williams2023-06-08T16:00:07Z UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of silsesquioxanes obtained by the hydrolytic condensation of (3-glycidoxypropyl)-trimethoxysilane in an epoxidized solvent Erra Balsells, Rosa (3 glycidoxypropyl)trimethoxysilane beta carboline silane derivative Silsesquioxane derivative solvent unclassified drug article chemical analysis chemical modification chemical reaction chemical structure epoxidation hydrolysis mass mass spectrometry matrix assisted laser desorption ionization time of flight mass spectrometry molecular stability polymerization reaction analysis synthesis Silsesquioxanes obtained by the bydrolytic condensation of (3-glycidoxypropyl)trimethoxysilane (GPMS) in diglycidyl ether of bisphenol A (DGEBA) were characterized by electraspray ionization time-of-flight mass spectrometry (ESI-TOF MS) and matrix-assisted ultraviolet laser desorption/ionizatian time-of-flight mass spectrometry (UV-MALDI-TOF MS), employing two different matrices and both positive and negative ion modes. A bimodal distribution of molar masses, in the 1300-6400 m/z range, was observed in MALDI mass spectra. This distribution accounted for oligomers formed in two successive generations but did not include a cluster of higher molar-mass species present in SEC chromatograms. Most of the peaks present in ESI and MALDI mass spectra could be described by the generic formula Tn(OCH3)m, with m = 0, 2, and 4 for n even, m = 1, 3, 5 for n = odd, and T = RSiO(3n-m)/2n. This corresponds to completely condensed polyhedra (m = 0), incompletely hydrolyzed polyhedra (m = 1 to 3), and their precursors (m = 4). Predominant species in the first cluster contained 10 to 14 Si atoms whereas those in the second cluster had 18 to 23 Si atoms. Small amounts of the following species: T8(OH)(OCH2), T9(OH), T10(OH)(OCH3), and T11(OH) could be identified in MALDI MS, using 9H-pyrido[3,4-b]indole (nor-harmane) as matrix in the I negative ion mode. It was inferred that some of these species had a relevant participation in the generation of the second cluster of higher molar masses. The stability of the silsesquioxane solution in DGEBA was the result of the very small concentration of free SiOH groups available for further condensation. © Wiley-VCH Verlag GmbH, 2001. Fil:Erra-Balsells, R. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales; Argentina. 2001 https://bibliotecadigital.exactas.uba.ar/collection/paper/document/paper_10221352_v202_n11_p2425_Williams http://hdl.handle.net/20.500.12110/paper_10221352_v202_n11_p2425_Williams
institution Universidad de Buenos Aires
institution_str I-28
repository_str R-134
collection Biblioteca Digital - Facultad de Ciencias Exactas y Naturales (UBA)
topic (3 glycidoxypropyl)trimethoxysilane
beta carboline
silane derivative
Silsesquioxane derivative
solvent
unclassified drug
article
chemical analysis
chemical modification
chemical reaction
chemical structure
epoxidation
hydrolysis
mass
mass spectrometry
matrix assisted laser desorption ionization time of flight mass spectrometry
molecular stability
polymerization
reaction analysis
synthesis
spellingShingle (3 glycidoxypropyl)trimethoxysilane
beta carboline
silane derivative
Silsesquioxane derivative
solvent
unclassified drug
article
chemical analysis
chemical modification
chemical reaction
chemical structure
epoxidation
hydrolysis
mass
mass spectrometry
matrix assisted laser desorption ionization time of flight mass spectrometry
molecular stability
polymerization
reaction analysis
synthesis
Erra Balsells, Rosa
UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of silsesquioxanes obtained by the hydrolytic condensation of (3-glycidoxypropyl)-trimethoxysilane in an epoxidized solvent
topic_facet (3 glycidoxypropyl)trimethoxysilane
beta carboline
silane derivative
Silsesquioxane derivative
solvent
unclassified drug
article
chemical analysis
chemical modification
chemical reaction
chemical structure
epoxidation
hydrolysis
mass
mass spectrometry
matrix assisted laser desorption ionization time of flight mass spectrometry
molecular stability
polymerization
reaction analysis
synthesis
description Silsesquioxanes obtained by the bydrolytic condensation of (3-glycidoxypropyl)trimethoxysilane (GPMS) in diglycidyl ether of bisphenol A (DGEBA) were characterized by electraspray ionization time-of-flight mass spectrometry (ESI-TOF MS) and matrix-assisted ultraviolet laser desorption/ionizatian time-of-flight mass spectrometry (UV-MALDI-TOF MS), employing two different matrices and both positive and negative ion modes. A bimodal distribution of molar masses, in the 1300-6400 m/z range, was observed in MALDI mass spectra. This distribution accounted for oligomers formed in two successive generations but did not include a cluster of higher molar-mass species present in SEC chromatograms. Most of the peaks present in ESI and MALDI mass spectra could be described by the generic formula Tn(OCH3)m, with m = 0, 2, and 4 for n even, m = 1, 3, 5 for n = odd, and T = RSiO(3n-m)/2n. This corresponds to completely condensed polyhedra (m = 0), incompletely hydrolyzed polyhedra (m = 1 to 3), and their precursors (m = 4). Predominant species in the first cluster contained 10 to 14 Si atoms whereas those in the second cluster had 18 to 23 Si atoms. Small amounts of the following species: T8(OH)(OCH2), T9(OH), T10(OH)(OCH3), and T11(OH) could be identified in MALDI MS, using 9H-pyrido[3,4-b]indole (nor-harmane) as matrix in the I negative ion mode. It was inferred that some of these species had a relevant participation in the generation of the second cluster of higher molar masses. The stability of the silsesquioxane solution in DGEBA was the result of the very small concentration of free SiOH groups available for further condensation. © Wiley-VCH Verlag GmbH, 2001.
author Erra Balsells, Rosa
author_facet Erra Balsells, Rosa
author_sort Erra Balsells, Rosa
title UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of silsesquioxanes obtained by the hydrolytic condensation of (3-glycidoxypropyl)-trimethoxysilane in an epoxidized solvent
title_short UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of silsesquioxanes obtained by the hydrolytic condensation of (3-glycidoxypropyl)-trimethoxysilane in an epoxidized solvent
title_full UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of silsesquioxanes obtained by the hydrolytic condensation of (3-glycidoxypropyl)-trimethoxysilane in an epoxidized solvent
title_fullStr UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of silsesquioxanes obtained by the hydrolytic condensation of (3-glycidoxypropyl)-trimethoxysilane in an epoxidized solvent
title_full_unstemmed UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of silsesquioxanes obtained by the hydrolytic condensation of (3-glycidoxypropyl)-trimethoxysilane in an epoxidized solvent
title_sort uv-maldi-tof and esi-tof mass spectrometry characterization of silsesquioxanes obtained by the hydrolytic condensation of (3-glycidoxypropyl)-trimethoxysilane in an epoxidized solvent
publishDate 2001
url https://bibliotecadigital.exactas.uba.ar/collection/paper/document/paper_10221352_v202_n11_p2425_Williams
http://hdl.handle.net/20.500.12110/paper_10221352_v202_n11_p2425_Williams
work_keys_str_mv AT errabalsellsrosa uvmalditofandesitofmassspectrometrycharacterizationofsilsesquioxanesobtainedbythehydrolyticcondensationof3glycidoxypropyltrimethoxysilaneinanepoxidizedsolvent
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