Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylate

Autores
Lambi, John N.; Nsehyuka, Alfred T.; Egbewatt, Nkongho; Cafferata, Lázaro F. R.; Arvia, Alejandro Jorge
Año de publicación
2003
Idioma
inglés
Tipo de recurso
artículo
Estado
versión publicada
Descripción
The thermal behaviour of zinc(II) acetylsalicylate [Zn(acsa)2(H2O)2] with respect to phase transitions, pyrolysis both in air and inert (N2) atmosphere, and product identification has been investigated. The complex was synthesised by metathesis in hot ethanol solution using aspirin (acetylsalicylic acid) as precursor and characterised via electronic and IR spectral analyses. Optical observations showed that the white salt does not undergo a direct transition from the solid to the liquid phase but rather goes slowly through an intermediate mesophase around 80 °C before melting rapidly to the brick-brown isotropic liquid around 134–136 °C. No liquid crystalline phases are however formed. This result was complemented by that from thermogravimetric (TG) studies in the ca. 25–600 °C range, which showed three main weight-loss phases of 8.0, 50.0 and 14.0% (around 200, 250 and 400 °C) corresponding, respectively, to the elimination of CO2, xanthone and acetic acid. The pyrolysis products, as identified using a combination of instrumental (GC–MS) and wet chemical techniques are: CO2; non-stoichiometric zinc oxide, most likely in the form: Zn1+xO (where 0.0000≤x≤0.0003); and a mixture of organic products resulting from further decomposition, charring and other attendant thermal effects at the relatively high temperatures (ca. 600 °C) involved. Six of the principal organic products were identified and included salsalate and benorylate which are pro-drugs of salicylic acid, a well-known pharmaceutical.
Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas
Materia
Ciencias Exactas
Química
Acetylsalicylate
Pyrolysis
Mesophase
Metathesis
Themogravimetry
Pro-drug
Precursor
Nivel de accesibilidad
acceso abierto
Condiciones de uso
http://creativecommons.org/licenses/by/4.0/
Repositorio
SEDICI (UNLP)
Institución
Universidad Nacional de La Plata
OAI Identificador
oai:sedici.unlp.edu.ar:10915/127494

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oai_identifier_str oai:sedici.unlp.edu.ar:10915/127494
network_acronym_str SEDICI
repository_id_str 1329
network_name_str SEDICI (UNLP)
spelling Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylateLambi, John N.Nsehyuka, Alfred T.Egbewatt, NkonghoCafferata, Lázaro F. R.Arvia, Alejandro JorgeCiencias ExactasQuímicaAcetylsalicylatePyrolysisMesophaseMetathesisThemogravimetryPro-drugPrecursorThe thermal behaviour of zinc(II) acetylsalicylate [Zn(acsa)<sub>2</sub>(H<sub>2</sub>O)<sub>2</sub>] with respect to phase transitions, pyrolysis both in air and inert (N<sub>2</sub>) atmosphere, and product identification has been investigated. The complex was synthesised by metathesis in hot ethanol solution using aspirin (acetylsalicylic acid) as precursor and characterised via electronic and IR spectral analyses. Optical observations showed that the white salt does not undergo a direct transition from the solid to the liquid phase but rather goes slowly through an intermediate mesophase around 80 °C before melting rapidly to the brick-brown isotropic liquid around 134–136 °C. No liquid crystalline phases are however formed. This result was complemented by that from thermogravimetric (TG) studies in the ca. 25–600 °C range, which showed three main weight-loss phases of 8.0, 50.0 and 14.0% (around 200, 250 and 400 °C) corresponding, respectively, to the elimination of CO<sub>2</sub>, xanthone and acetic acid. The pyrolysis products, as identified using a combination of instrumental (GC–MS) and wet chemical techniques are: CO<sub>2</sub>; non-stoichiometric zinc oxide, most likely in the form: Zn<sub>1+x</sub>O (where 0.0000≤x≤0.0003); and a mixture of organic products resulting from further decomposition, charring and other attendant thermal effects at the relatively high temperatures (ca. 600 °C) involved. Six of the principal organic products were identified and included salsalate and benorylate which are pro-drugs of salicylic acid, a well-known pharmaceutical.Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas2003info:eu-repo/semantics/articleinfo:eu-repo/semantics/publishedVersionArticulohttp://purl.org/coar/resource_type/c_6501info:ar-repo/semantics/articuloapplication/pdf145-151http://sedici.unlp.edu.ar/handle/10915/127494enginfo:eu-repo/semantics/altIdentifier/url/https://www.sciencedirect.com/science/article/abs/pii/S0040603102003544info:eu-repo/semantics/altIdentifier/issn/0040-6031info:eu-repo/semantics/altIdentifier/doi/10.1016/S0040-6031(02)00354-4info:eu-repo/semantics/openAccesshttp://creativecommons.org/licenses/by/4.0/Creative Commons Attribution 4.0 International (CC BY 4.0)reponame:SEDICI (UNLP)instname:Universidad Nacional de La Platainstacron:UNLP2025-09-29T11:30:48Zoai:sedici.unlp.edu.ar:10915/127494Institucionalhttp://sedici.unlp.edu.ar/Universidad públicaNo correspondehttp://sedici.unlp.edu.ar/oai/snrdalira@sedici.unlp.edu.arArgentinaNo correspondeNo correspondeNo correspondeopendoar:13292025-09-29 11:30:48.994SEDICI (UNLP) - Universidad Nacional de La Platafalse
dc.title.none.fl_str_mv Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylate
title Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylate
spellingShingle Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylate
Lambi, John N.
Ciencias Exactas
Química
Acetylsalicylate
Pyrolysis
Mesophase
Metathesis
Themogravimetry
Pro-drug
Precursor
title_short Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylate
title_full Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylate
title_fullStr Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylate
title_full_unstemmed Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylate
title_sort Synthesis, spectral properties and thermal behaviour of zinc(II) acetylsalicylate
dc.creator.none.fl_str_mv Lambi, John N.
Nsehyuka, Alfred T.
Egbewatt, Nkongho
Cafferata, Lázaro F. R.
Arvia, Alejandro Jorge
author Lambi, John N.
author_facet Lambi, John N.
Nsehyuka, Alfred T.
Egbewatt, Nkongho
Cafferata, Lázaro F. R.
Arvia, Alejandro Jorge
author_role author
author2 Nsehyuka, Alfred T.
Egbewatt, Nkongho
Cafferata, Lázaro F. R.
Arvia, Alejandro Jorge
author2_role author
author
author
author
dc.subject.none.fl_str_mv Ciencias Exactas
Química
Acetylsalicylate
Pyrolysis
Mesophase
Metathesis
Themogravimetry
Pro-drug
Precursor
topic Ciencias Exactas
Química
Acetylsalicylate
Pyrolysis
Mesophase
Metathesis
Themogravimetry
Pro-drug
Precursor
dc.description.none.fl_txt_mv The thermal behaviour of zinc(II) acetylsalicylate [Zn(acsa)<sub>2</sub>(H<sub>2</sub>O)<sub>2</sub>] with respect to phase transitions, pyrolysis both in air and inert (N<sub>2</sub>) atmosphere, and product identification has been investigated. The complex was synthesised by metathesis in hot ethanol solution using aspirin (acetylsalicylic acid) as precursor and characterised via electronic and IR spectral analyses. Optical observations showed that the white salt does not undergo a direct transition from the solid to the liquid phase but rather goes slowly through an intermediate mesophase around 80 °C before melting rapidly to the brick-brown isotropic liquid around 134–136 °C. No liquid crystalline phases are however formed. This result was complemented by that from thermogravimetric (TG) studies in the ca. 25–600 °C range, which showed three main weight-loss phases of 8.0, 50.0 and 14.0% (around 200, 250 and 400 °C) corresponding, respectively, to the elimination of CO<sub>2</sub>, xanthone and acetic acid. The pyrolysis products, as identified using a combination of instrumental (GC–MS) and wet chemical techniques are: CO<sub>2</sub>; non-stoichiometric zinc oxide, most likely in the form: Zn<sub>1+x</sub>O (where 0.0000≤x≤0.0003); and a mixture of organic products resulting from further decomposition, charring and other attendant thermal effects at the relatively high temperatures (ca. 600 °C) involved. Six of the principal organic products were identified and included salsalate and benorylate which are pro-drugs of salicylic acid, a well-known pharmaceutical.
Instituto de Investigaciones Fisicoquímicas Teóricas y Aplicadas
description The thermal behaviour of zinc(II) acetylsalicylate [Zn(acsa)<sub>2</sub>(H<sub>2</sub>O)<sub>2</sub>] with respect to phase transitions, pyrolysis both in air and inert (N<sub>2</sub>) atmosphere, and product identification has been investigated. The complex was synthesised by metathesis in hot ethanol solution using aspirin (acetylsalicylic acid) as precursor and characterised via electronic and IR spectral analyses. Optical observations showed that the white salt does not undergo a direct transition from the solid to the liquid phase but rather goes slowly through an intermediate mesophase around 80 °C before melting rapidly to the brick-brown isotropic liquid around 134–136 °C. No liquid crystalline phases are however formed. This result was complemented by that from thermogravimetric (TG) studies in the ca. 25–600 °C range, which showed three main weight-loss phases of 8.0, 50.0 and 14.0% (around 200, 250 and 400 °C) corresponding, respectively, to the elimination of CO<sub>2</sub>, xanthone and acetic acid. The pyrolysis products, as identified using a combination of instrumental (GC–MS) and wet chemical techniques are: CO<sub>2</sub>; non-stoichiometric zinc oxide, most likely in the form: Zn<sub>1+x</sub>O (where 0.0000≤x≤0.0003); and a mixture of organic products resulting from further decomposition, charring and other attendant thermal effects at the relatively high temperatures (ca. 600 °C) involved. Six of the principal organic products were identified and included salsalate and benorylate which are pro-drugs of salicylic acid, a well-known pharmaceutical.
publishDate 2003
dc.date.none.fl_str_mv 2003
dc.type.none.fl_str_mv info:eu-repo/semantics/article
info:eu-repo/semantics/publishedVersion
Articulo
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://sedici.unlp.edu.ar/handle/10915/127494
url http://sedici.unlp.edu.ar/handle/10915/127494
dc.language.none.fl_str_mv eng
language eng
dc.relation.none.fl_str_mv info:eu-repo/semantics/altIdentifier/url/https://www.sciencedirect.com/science/article/abs/pii/S0040603102003544
info:eu-repo/semantics/altIdentifier/issn/0040-6031
info:eu-repo/semantics/altIdentifier/doi/10.1016/S0040-6031(02)00354-4
dc.rights.none.fl_str_mv info:eu-repo/semantics/openAccess
http://creativecommons.org/licenses/by/4.0/
Creative Commons Attribution 4.0 International (CC BY 4.0)
eu_rights_str_mv openAccess
rights_invalid_str_mv http://creativecommons.org/licenses/by/4.0/
Creative Commons Attribution 4.0 International (CC BY 4.0)
dc.format.none.fl_str_mv application/pdf
145-151
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instname:Universidad Nacional de La Plata
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reponame_str SEDICI (UNLP)
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instname_str Universidad Nacional de La Plata
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