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Coupling HPLC and GC-FID for the monitorization of oxidized intermediates from wet peroxide biphasic oxidation

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dc.contributor.authorDíaz de Tuesta, Jose Luis
dc.contributor.authorAmaral, Joana S.
dc.contributor.authorSilva, Adrián
dc.contributor.authorFaria, Joaquim
dc.contributor.authorGomes, Helder
dc.date.accessioned2020-07-14T08:22:10Z
dc.date.available2020-07-14T08:22:10Z
dc.date.issued2017
dc.description.abstractA GC-FID method capable to detect 2-nitrophenol (2-NP) and the resulting intermediates from its oxidation with H2O2 was developed and validated under the typical criteria for in-house pre-validation [1]. Linearity was demonstrated by F-test; accuracy and precision were assessed in three concentration levels. The oxidation process under study consists on the peroxidation of 2-NP, used as target lipophilic pollutant, in a biphasic mixture of cyclohexane(cC6)/water to simulate contaminated oily streams. The oxidized intermediates produced by the peroxidation of 2-NP (POW = 51.3) in aqueous phase are phenol (Ph, POW = 30.2), hydroquinone (HQ, POW = 4.4), p-benzoquinone (BQ, POW = 1.9), catechol (CTL, POW = 7.6) and carboxylic acids [1]. Those compounds can be quantified in the aqueous phase by previous developed HPLC methods [2]. In the biphasic medium of reaction, the oxidation of cC6 can also take place to produce cyclohexanone (cC6O, POW = 5.8) and cyclohexanol (cC6OH, POW = 21.9). The cC6- water partition coefficient of 2-NP and the oxidized cyclic intermediates, a priori all lipophilic compounds, were assessed by analysis of the aqueous phase before and after addition of different volumes of cC6. HQ and CTL keep their concentration in the aqueous phase after cC6 addition and only the analysis of the other analytes (dissolved in cC6) were done by GC-FID (Scion 436-GC, Bruker), without derivatization and adding a little quantity of Na2SO4 to remove the moisture. The injector and detector temperatures were set at 260 ºC and 270ºC, respectively. Separation was performed on a 50 m x 0.25 mm CP-Sil 88 column using the following temperature program: a first isotherm step at 160 ºC, followed by a heating ramp at 5 ºC/min, then at 10 ºC/min and a final isotherm step at 220 ºC during 5, 2, 5 and 5 min, respectively. At these conditions, the cC6, cC6O, cC6OH, BQ, 2-NP and Ph compounds show well resolved peaks, and the method is capable to detect the compounds with maximum concentrations of 4.7, 2.3, 1.3, 1.0 and 7.1 g/L (in the same order) without overlap. The developed method, coupled with the HPLC methods, allows to follow the evolution of all compounds in the biphasic oxidation system.pt_PT
dc.description.sponsorshipThis work is a result of project “AIProcMat@N2020 - Advanced Industrial Processes and Materials for a Sustainable Northern Region of Portugal 2020”, with the reference NORTE-01-0145-FEDER-000006, supported by NORTE 2020, under the Portugal 2020 Partnership Agreement, through FEDER and of Project POCI-01-0145-FEDER-006984 – Associate Laboratory LSRE-LCM funded by FEDER through COMPETE2020 - POCI – and by national funds through FCT. A.M.T. Silva acknowledges the FCT Investigator 2013 Programme (IF/01501/2013), with financing from the European Social Fund and the Human Potential Operational Programme.pt_PT
dc.description.versioninfo:eu-repo/semantics/publishedVersionpt_PT
dc.identifier.citationDíaz de Tuesta, Jose Luis; Amaral, J.S.; Silva, Adrián; Faria, Joaquim; Gomes, Helder (2017). Coupling HPLC and GC-FID for the monitorization of oxidized intermediates from wet peroxide biphasic oxidation. In 10º Encontro Nacional de Cromatografia. Bragança. ISBN 978-972-745-234-7pt_PT
dc.identifier.isbn978-972-745-234-7
dc.identifier.urihttp://hdl.handle.net/10198/22467
dc.language.isoengpt_PT
dc.peerreviewedyespt_PT
dc.rights.urihttp://creativecommons.org/licenses/by-nc/4.0/pt_PT
dc.titleCoupling HPLC and GC-FID for the monitorization of oxidized intermediates from wet peroxide biphasic oxidationpt_PT
dc.typeconference object
dspace.entity.typePublication
oaire.citation.conferencePlaceBragança, Portugalpt_PT
oaire.citation.endPage119pt_PT
oaire.citation.startPage119pt_PT
oaire.citation.title10º Encontro Nacional de Cromatografiapt_PT
person.familyNameDíaz de Tuesta
person.familyNameAmaral
person.familyNameGomes
person.givenNameJose Luis
person.givenNameJoana S.
person.givenNameHelder
person.identifier.ciencia-id7A1F-022B-7DBF
person.identifier.ciencia-id5319-7DE8-BEDA
person.identifier.ciencia-id6218-1E19-13EE
person.identifier.orcid0000-0003-2408-087X
person.identifier.orcid0000-0002-3648-7303
person.identifier.orcid0000-0001-6898-2408
person.identifier.ridD-9785-2017
person.identifier.scopus-author-id55755821600
rcaap.rightsopenAccesspt_PT
rcaap.typeconferenceObjectpt_PT
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relation.isAuthorOfPublication42be2cf4-adc4-4e7f-ac60-7aab515b38cd
relation.isAuthorOfPublication0eb96337-224a-4339-9918-334436fbbb99
relation.isAuthorOfPublication.latestForDiscovery0eb96337-224a-4339-9918-334436fbbb99

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