One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products

Autores
Fasce, Diana Patricia; Williams, Roberto Juan Jose; Erra Balsells, Rosa; Ishikawa, Yoko; Nonami, Hiroshi
Año de publicación
2001
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
The NaOH-catalyzed hydrolytic condensation of the reaction product between N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and phenyl glycidyl ether (PGE) was followed by matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry (UV-MALDI-TOF MS) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF MS). After 24 h at 50 °C, main condensation products were a mixture of perfect and imperfect polyhedra:  T8, T9(OH), and T10, with traces of T7(OH) and T11(OH). Every one of these products was composed of a series of peaks in the mass spectra, accounting for the incomplete reaction of PGE with the aminosilane (e.g., T8 showed the presence of the species containing 24 PGE units arising from the complete reaction of the initial silane, as well as species containing 23, 22, and 21 PGE units). A thermal treatment to 150 °C led to the appearance of extra peaks corresponding to intramolecular dehydration products. Peaks corresponding to the loss of one water molecule from T9(OH) and T7(OH) were present and could be ascribed to the reaction between SiOH and a secondary OH group. Dehydration products from T8 and T10 were observed, as well as species arising from the loss of two water molecules from T9(OH) and T7(OH). A plausible explanation for the presence of these peaks is the rupture of a Si−O−Si bond in the presence of NaOH, followed by condensation of the resulting fragments with secondary OH groups.
Fil: Fasce, Diana Patricia. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Williams, Roberto Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Erra Balsells, Rosa. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Ciudad Universitaria. Centro de Investigaciones en Hidratos de Carbono. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales. Centro de Investigaciones en Hidratos de Carbono; Argentina
Fil: Ishikawa, Yoko. Ehime University; Japón
Fil: Nonami, Hiroshi. Ehime University; Japón
Materia
Polyhedral Silsesquioxanes
Hydrolytic Condensation
Uv-Maldi-Tof Ms
Nivel de accesibilidad
acceso abierto
Condiciones de uso
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
Repositorio
CONICET Digital (CONICET)
Institución
Consejo Nacional de Investigaciones Científicas y Técnicas
OAI Identificador
oai:ri.conicet.gov.ar:11336/35607
Acceder
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oai_identifier_str oai:ri.conicet.gov.ar:11336/35607
network_acronym_str CONICETDig
repository_id_str 3498
network_name_str CONICET Digital (CONICET)
spelling One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction productsFasce, Diana PatriciaWilliams, Roberto Juan JoseErra Balsells, RosaIshikawa, YokoNonami, HiroshiPolyhedral SilsesquioxanesHydrolytic CondensationUv-Maldi-Tof Mshttps://purl.org/becyt/ford/1.4https://purl.org/becyt/ford/1The NaOH-catalyzed hydrolytic condensation of the reaction product between N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and phenyl glycidyl ether (PGE) was followed by matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry (UV-MALDI-TOF MS) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF MS). After 24 h at 50 °C, main condensation products were a mixture of perfect and imperfect polyhedra:  T8, T9(OH), and T10, with traces of T7(OH) and T11(OH). Every one of these products was composed of a series of peaks in the mass spectra, accounting for the incomplete reaction of PGE with the aminosilane (e.g., T8 showed the presence of the species containing 24 PGE units arising from the complete reaction of the initial silane, as well as species containing 23, 22, and 21 PGE units). A thermal treatment to 150 °C led to the appearance of extra peaks corresponding to intramolecular dehydration products. Peaks corresponding to the loss of one water molecule from T9(OH) and T7(OH) were present and could be ascribed to the reaction between SiOH and a secondary OH group. Dehydration products from T8 and T10 were observed, as well as species arising from the loss of two water molecules from T9(OH) and T7(OH). A plausible explanation for the presence of these peaks is the rupture of a Si−O−Si bond in the presence of NaOH, followed by condensation of the resulting fragments with secondary OH groups.Fil: Fasce, Diana Patricia. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaFil: Williams, Roberto Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; ArgentinaFil: Erra Balsells, Rosa. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Ciudad Universitaria. Centro de Investigaciones en Hidratos de Carbono. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales. Centro de Investigaciones en Hidratos de Carbono; ArgentinaFil: Ishikawa, Yoko. Ehime University; JapónFil: Nonami, Hiroshi. Ehime University; JapónAmerican Chemical Society2001-04-19info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionhttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdfapplication/pdfhttp://hdl.handle.net/11336/35607Fasce, Diana Patricia; Williams, Roberto Juan Jose; Erra Balsells, Rosa; Ishikawa, Yoko; Nonami, Hiroshi; One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products; American Chemical Society; Macromolecules; 34; 11; 19-4-2001; 3534-35390024-9297CONICET DigitalCONICETenginfo:eu-repo/semantics/altIdentifier/url/https://pubs.acs.org/doi/abs/10.1021/ma001711kinfo:eu-repo/semantics/altIdentifier/doi/10.1021/ma001711kinfo:eu-repo/semantics/openAccesshttps://creativecommons.org/licenses/by-nc-sa/2.5/ar/reponame:CONICET Digital (CONICET)instname:Consejo Nacional de Investigaciones Científicas y Técnicas2025-09-29T09:33:27Zoai:ri.conicet.gov.ar:11336/35607instacron:CONICETInstitucionalhttp://ri.conicet.gov.ar/Organismo científico-tecnológicoNo correspondehttp://ri.conicet.gov.ar/oai/requestdasensio@conicet.gov.ar; lcarlino@conicet.gov.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:34982025-09-29 09:33:27.983CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicasfalse
dc.title.none.fl_str_mv One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
spellingShingle One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
Fasce, Diana Patricia
Polyhedral Silsesquioxanes
Hydrolytic Condensation
Uv-Maldi-Tof Ms
title_short One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title_full One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title_fullStr One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title_full_unstemmed One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
title_sort One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products
dc.creator.none.fl_str_mv Fasce, Diana Patricia
Williams, Roberto Juan Jose
Erra Balsells, Rosa
Ishikawa, Yoko
Nonami, Hiroshi
author Fasce, Diana Patricia
author_facet Fasce, Diana Patricia
Williams, Roberto Juan Jose
Erra Balsells, Rosa
Ishikawa, Yoko
Nonami, Hiroshi
author_role author
author2 Williams, Roberto Juan Jose
Erra Balsells, Rosa
Ishikawa, Yoko
Nonami, Hiroshi
author2_role author
author
author
author
dc.subject.none.fl_str_mv Polyhedral Silsesquioxanes
Hydrolytic Condensation
Uv-Maldi-Tof Ms
topic Polyhedral Silsesquioxanes
Hydrolytic Condensation
Uv-Maldi-Tof Ms
purl_subject.fl_str_mv https://purl.org/becyt/ford/1.4
https://purl.org/becyt/ford/1
dc.description.none.fl_txt_mv The NaOH-catalyzed hydrolytic condensation of the reaction product between N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and phenyl glycidyl ether (PGE) was followed by matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry (UV-MALDI-TOF MS) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF MS). After 24 h at 50 °C, main condensation products were a mixture of perfect and imperfect polyhedra:  T8, T9(OH), and T10, with traces of T7(OH) and T11(OH). Every one of these products was composed of a series of peaks in the mass spectra, accounting for the incomplete reaction of PGE with the aminosilane (e.g., T8 showed the presence of the species containing 24 PGE units arising from the complete reaction of the initial silane, as well as species containing 23, 22, and 21 PGE units). A thermal treatment to 150 °C led to the appearance of extra peaks corresponding to intramolecular dehydration products. Peaks corresponding to the loss of one water molecule from T9(OH) and T7(OH) were present and could be ascribed to the reaction between SiOH and a secondary OH group. Dehydration products from T8 and T10 were observed, as well as species arising from the loss of two water molecules from T9(OH) and T7(OH). A plausible explanation for the presence of these peaks is the rupture of a Si−O−Si bond in the presence of NaOH, followed by condensation of the resulting fragments with secondary OH groups.
Fil: Fasce, Diana Patricia. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Williams, Roberto Juan Jose. Consejo Nacional de Investigaciones Científicas y Técnicas. Centro Científico Tecnológico Conicet - Mar del Plata. Instituto de Investigaciones en Ciencia y Tecnología de Materiales. Universidad Nacional de Mar del Plata. Facultad de Ingeniería. Instituto de Investigaciones en Ciencia y Tecnología de Materiales; Argentina
Fil: Erra Balsells, Rosa. Consejo Nacional de Investigaciones Científicas y Técnicas. Oficina de Coordinación Administrativa Ciudad Universitaria. Centro de Investigaciones en Hidratos de Carbono. Universidad de Buenos Aires. Facultad de Ciencias Exactas y Naturales. Centro de Investigaciones en Hidratos de Carbono; Argentina
Fil: Ishikawa, Yoko. Ehime University; Japón
Fil: Nonami, Hiroshi. Ehime University; Japón
description The NaOH-catalyzed hydrolytic condensation of the reaction product between N-(β-aminoethyl)-γ-aminopropyltrimethoxysilane and phenyl glycidyl ether (PGE) was followed by matrix-assisted ultraviolet laser desorption/ionization time-of-flight mass spectrometry (UV-MALDI-TOF MS) and electrospray ionization time-of-flight mass spectrometry (ESI-TOF MS). After 24 h at 50 °C, main condensation products were a mixture of perfect and imperfect polyhedra:  T8, T9(OH), and T10, with traces of T7(OH) and T11(OH). Every one of these products was composed of a series of peaks in the mass spectra, accounting for the incomplete reaction of PGE with the aminosilane (e.g., T8 showed the presence of the species containing 24 PGE units arising from the complete reaction of the initial silane, as well as species containing 23, 22, and 21 PGE units). A thermal treatment to 150 °C led to the appearance of extra peaks corresponding to intramolecular dehydration products. Peaks corresponding to the loss of one water molecule from T9(OH) and T7(OH) were present and could be ascribed to the reaction between SiOH and a secondary OH group. Dehydration products from T8 and T10 were observed, as well as species arising from the loss of two water molecules from T9(OH) and T7(OH). A plausible explanation for the presence of these peaks is the rupture of a Si−O−Si bond in the presence of NaOH, followed by condensation of the resulting fragments with secondary OH groups.
publishDate 2001
dc.date.none.fl_str_mv 2001-04-19
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
http://purl.org/coar/resource_type/c_6501
info:ar-repo/semantics/articulo
format article
status_str publishedVersion
dc.identifier.none.fl_str_mv http://hdl.handle.net/11336/35607
Fasce, Diana Patricia; Williams, Roberto Juan Jose; Erra Balsells, Rosa; Ishikawa, Yoko; Nonami, Hiroshi; One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products; American Chemical Society; Macromolecules; 34; 11; 19-4-2001; 3534-3539
0024-9297
CONICET Digital
CONICET
url http://hdl.handle.net/11336/35607
identifier_str_mv Fasce, Diana Patricia; Williams, Roberto Juan Jose; Erra Balsells, Rosa; Ishikawa, Yoko; Nonami, Hiroshi; One-step synthesis of polyhedral silsesquioxanes bearing bulky substituents: UV-MALDI-TOF and ESI-TOF mass spectrometry characterization of reaction products; American Chemical Society; Macromolecules; 34; 11; 19-4-2001; 3534-3539
0024-9297
CONICET Digital
CONICET
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/url/https://pubs.acs.org/doi/abs/10.1021/ma001711k
info:eu-repo/semantics/altIdentifier/doi/10.1021/ma001711k
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
eu_rights_str_mv openAccess
rights_invalid_str_mv https://creativecommons.org/licenses/by-nc-sa/2.5/ar/
dc.format.none.fl_str_mv application/pdf
application/pdf
dc.publisher.none.fl_str_mv American Chemical Society
publisher.none.fl_str_mv American Chemical Society
dc.source.none.fl_str_mv reponame:CONICET Digital (CONICET)
instname:Consejo Nacional de Investigaciones Científicas y Técnicas
reponame_str CONICET Digital (CONICET)
collection CONICET Digital (CONICET)
instname_str Consejo Nacional de Investigaciones Científicas y Técnicas
repository.name.fl_str_mv CONICET Digital (CONICET) - Consejo Nacional de Investigaciones Científicas y Técnicas
repository.mail.fl_str_mv dasensio@conicet.gov.ar; lcarlino@conicet.gov.ar
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score 13.069144

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