mycoreobjectrosdok_disshab_0000003287rosdok_disshab_0000003287rosdokdisshabrosdok_derivate_00002250982025-07-21T13:40:31.721Z2025-07-21T13:14:54.948ZMCRJANITOReditorFGpublished1rosdok_derivate_0000225098truetruederivate_types:fulltextVolltextfulltextwf_edit_epub wf_register_epubstate:publishedstate:publishedveröffentlichtpublishedrosdok/id000048761931401799Oau2025-07-212025-07-21T13:30:25ZrdaConverted from PICA to MODS using Pica2MODS XSLT Transformer 2.10 [SCM: "f6c168af690edb7cb65ef34e4a2bf7f8714c5d38" "v2.10" "2024-03-28T14:43:08+0100"] with mode 'DEFAULT'.DissertationHochschulschriftDevelopment of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistryBenchtop low-field (LF) NMR spectroscopy is a valuable tool for reaction monitoring and its application in catalysis. It is particularly attractive thanks to its low-cost and portability (i.e., the instrument can be installed right next to the fume hood). However, crucial quantitative results, e.g., kinetic profiles, cannot be correctly determined the moment degradation of an air- and moisture-sensitive catalyst occurs. Therefore, inertness of the entire setup must be guaranteed. In the first part of this thesis, it is demonstrated that this challenge could be overcome to meet the experimental requirements of highly oxygen-sensitive rhodium diphosphine complexes, relevant for homogeneous catalysis. Indeed, a commercially available benchtop LF NMR spectrometer has been evolved into an inert customized flow setup. Catalytic hydrogenation monitoring via LF 1H and 31P NMR spectroscopy proved to be suitable with this flow setup despite the relatively low concentration of the investigated species (ca. 10 mM). In the second part of the thesis, limitations due to the low magnetic field of the benchtop spectrometer (1.9 T) and the relative insensitivity of 31P compared to 1H nucleus have been faced. 31P NMR signal-to-noise ratios (SNRs) have been improved using advanced pulse sequences. Sensitive Homogeneous And Resolved PEaks in Real time (SHARPER) enhances 31P NMR signals by collapsing the target resonance into an extremely narrow singlet and eliminating the effects of field inhomogeneity. After demonstrating the advantage of this tool in static conditions (up to 10-fold enhancement factor on SNR), the customized on-line setup has been used to monitor a faster reaction (in the order of minutes), that could not be followed with traditional 31P NMR sequences.LauraTadiello1996 -VerfasserInaut1372035028TorstenBeweries1982 -AkademischeR BetreuerIndgs1363494470000-0002-2416-8874Leibniz-Institut für Katalyse e. V.BjörnCorzilius1979 -AkademischeR BetreuerIndgs135774721Universität Rostock, Institut für Chemie38329-6Universität Rostock1419 - 19761990 -Grad-verleihende Institutiondgg2147083-2Universität Rostock. Mathematisch-Naturwissenschaftliche FakultätGrad-verleihende Institutiondgghttps://purl.uni-rostock.de/rosdok/id00004876urn:nbn:de:gbv:28-rosdok_id00004876-110.18453/rosdok_id00004876540 ChemieMathematisch-Naturwissenschaftliche Fakultätalle Rechte vorbehaltenNutzungsrechte erteiltLizenz Metadaten: CC0frei zugänglich (Open Access)en2024Universität RostockRostockmonographic202420242025Universitätsbibliothek RostockRostock2025Universitätsbibliothek Rostockhttps://purl.uni-rostock.de/rosdok/id00004876Torsten Beweries (Leibniz-Institut für Katalyse e. V.) ; Björn Corzilius (Universität Rostock, Institut für Chemie)[{"name":"Beweries, Torsten","affil":"Leibniz-Institut für Katalyse e. V."},{"name":"Corzilius, Björn","affil":"Universität Rostock, Institut für Chemie"}]Dissertation, Universität Rostock, 2024Nuclear magnetic resonancevorgelegt von Laura TadielloBeweries, TorstenLeibniz-Institut für Katalyse e. V.Corzilius, BjörnUniversität Rostock, Institut für Chemiedoctype:epubdoctype:epubDokumenttypDocument typedoctype:epub.dissertationdoctype:epub.dissertationDissertationdoctoral thesisdiniPublType:doctoralThesis diniPublType2022:PhDThesis XMetaDissPlusThesisLevel:thesis.doctoralinfo:eu-repo/semantics/doctoralThesisdocumentnatureOfContent:ppn_105825778natureOfContent:ppn_105825778HochschulschriftdiniPublType2022:DoctoralThesisdiniPublType2022:DoctoralThesisDissertation oder HabilitationDoctoral thesisDRIVERdiniPublType2022:PhDThesisdiniPublType2022:PhDThesisDissertationPhD thesisKDSF (Pu34)XMetaDissPlusThesisLevel:thesis.doctoralXMetaDissPlusThesisLevel:thesis.doctoralDoktorarbeitdoctoral thesisSDNB:540SDNB:540540 Chemie540 Chemistry & allied sciencesinstitution:unirostockinstitution:unirostockUniversität RostockUniversity of RostockUniversität RostockUniversität RostockUni.Rostockhttp://d-nb.info/gnd/38329-6institution:unirostock.mnfinstitution:unirostock.mnfMathematisch-Naturwissenschaftliche FakultätFaculty of Mathematics and Natural SciencesUniversität Rostock. Mathematisch-Naturwissenschaftliche FakultätMathematisch-Natur-<br />wissenschaftliche FakultätUni.Rostock.Fakultaet.MNFhttp://d-nb.info/gnd/2147083-2licenseinfo:worklicenseinfo:workWerkworklicenseinfo:work.rightsreservedlicenseinfo:work.rightsreservedalle Rechte vorbehaltenall rights reserved/creativecommons/r/reserved/0.9/88x31.png[DE-28]Urheberrechtsschutz 1.0$gRights Statements$uhttp://rightsstatements.org/vocab/InC/1.0/http://rightsstatements.org/vocab/InC/1.0/http://rightsstatements.org/vocab/InC/1.0/licenseinfo:depositlicenseinfo:depositVeröffentlichungsgenehmigungpermission to storelicenseinfo:deposit.rightsgrantedlicenseinfo:deposit.rightsgrantedNutzungsrechte erteiltrights grantedlicenseinfo:metadatalicenseinfo:metadataLizenzen für Metadatenlicenseinfo:metadata.cc0licenseinfo:metadata.cc0Lizenz Metadaten: CC0license metadata: CC0/creativecommons/p/zero/1.0/88x31.pnghttps://creativecommons.org/publicdomain/zero/1.0/accesscondition:openaccessaccesscondition:openaccessfrei zugänglich (Open Access)open accesshttp://purl.org/coar/access_right/c_abf2OAfreeinfo:eu-repo/semantics/openAccess[DE-28]Open Access$gControlled Vocabulary for Access Rights$uhttp://purl.org/coar/access_right/c_abf2rfc5646:enrfc5646:enEnglischEnglishengengDevelopment of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistryDevelopment of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistrygnd:1372035028gnd:136349447orcid:0000-0002-2416-8874gnd:135774721gnd:38329-6gnd:2147083-2gnd:1372035028gnd:136349447orcid:0000-0002-2416-8874gnd:135774721gnd:38329-6gnd:2147083-2rosdok_disshab_0000003287-d598161e52gnd:1372035028Laura TadielloLaura Tadiellorosdok_disshab_0000003287-d598161e66gnd:136349447orcid:0000-0002-2416-8874Torsten BeweriesTorsten Beweriesrosdok_disshab_0000003287-d598161e83gnd:135774721Björn CorziliusBjörn Corziliusrosdok_disshab_0000003287-d598161e98gnd:38329-6Universität RostockUniversität Rostockrosdok_disshab_0000003287-d598161e112gnd:2147083-2Universität Rostock. Mathematisch-Naturwissenschaftliche FakultätUniversität Rostock. Mathematisch-Naturwissenschaftliche FakultätLaura TadielloTorsten BeweriesBjörn CorziliusUniversität RostockUniversität Rostock. Mathematisch-Naturwissenschaftliche FakultätLaura TadielloTorsten BeweriesBjörn CorziliusUniversität RostockUniversität Rostock. Mathematisch-Naturwissenschaftliche FakultätLaura TadielloRostockUniversität Rostockepub.dissertationhttps://purl.uni-rostock.de/rosdok/id00004876urn:nbn:de:gbv:28-rosdok_id00004876-110.18453/rosdok_id00004876Benchtop low-field (LF) NMR spectroscopy is a valuable tool for reaction monitoring and its application in catalysis. It is particularly attractive thanks to its low-cost and portability (i.e., the instrument can be installed right next to the fume hood). However, crucial quantitative results, e.g., kinetic profiles, cannot be correctly determined the moment degradation of an air- and moisture-sensitive catalyst occurs. Therefore, inertness of the entire setup must be guaranteed. In the first part of this thesis, it is demonstrated that this challenge could be overcome to meet the experimental requirements of highly oxygen-sensitive rhodium diphosphine complexes, relevant for homogeneous catalysis. Indeed, a commercially available benchtop LF NMR spectrometer has been evolved into an inert customized flow setup. Catalytic hydrogenation monitoring via LF 1H and 31P NMR spectroscopy proved to be suitable with this flow setup despite the relatively low concentration of the investigated species (ca. 10 mM). In the second part of the thesis, limitations due to the low magnetic field of the benchtop spectrometer (1.9 T) and the relative insensitivity of 31P compared to 1H nucleus have been faced. 31P NMR signal-to-noise ratios (SNRs) have been improved using advanced pulse sequences. Sensitive Homogeneous And Resolved PEaks in Real time (SHARPER) enhances 31P NMR signals by collapsing the target resonance into an extremely narrow singlet and eliminating the effects of field inhomogeneity. After demonstrating the advantage of this tool in static conditions (up to 10-fold enhancement factor on SNR), the customized on-line setup has been used to monitor a faster reaction (in the order of minutes), that could not be followed with traditional 31P NMR sequences.20242024Torsten Beweries (Leibniz-Institut für Katalyse e. V.) ; Björn Corzilius (Universität Rostock, Institut für Chemie)[{"name":"Beweries, Torsten","affil":"Leibniz-Institut für Katalyse e. V."},{"name":"Corzilius, Björn","affil":"Universität Rostock, Institut für Chemie"}]Dissertation, Universität Rostock, 2024Nuclear magnetic resonancevorgelegt von Laura Tadielloepub.dissertation1 Tadiello_Dissertation_2025.pdf 6478533 3d027dcd69cd4caabde5298a8d62793b rosdok/id000048761931401799Oau2025-07-212025-07-21T13:30:25ZrdaConverted from PICA to MODS using Pica2MODS XSLT Transformer 2.10 [SCM: "f6c168af690edb7cb65ef34e4a2bf7f8714c5d38" "v2.10" "2024-03-28T14:43:08+0100"] with mode 'DEFAULT'.DissertationHochschulschriftDevelopment of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistryBenchtop low-field (LF) NMR spectroscopy is a valuable tool for reaction monitoring and its application in catalysis. It is particularly attractive thanks to its low-cost and portability (i.e., the instrument can be installed right next to the fume hood). However, crucial quantitative results, e.g., kinetic profiles, cannot be correctly determined the moment degradation of an air- and moisture-sensitive catalyst occurs. Therefore, inertness of the entire setup must be guaranteed. In the first part of this thesis, it is demonstrated that this challenge could be overcome to meet the experimental requirements of highly oxygen-sensitive rhodium diphosphine complexes, relevant for homogeneous catalysis. Indeed, a commercially available benchtop LF NMR spectrometer has been evolved into an inert customized flow setup. Catalytic hydrogenation monitoring via LF 1H and 31P NMR spectroscopy proved to be suitable with this flow setup despite the relatively low concentration of the investigated species (ca. 10 mM). In the second part of the thesis, limitations due to the low magnetic field of the benchtop spectrometer (1.9 T) and the relative insensitivity of 31P compared to 1H nucleus have been faced. 31P NMR signal-to-noise ratios (SNRs) have been improved using advanced pulse sequences. Sensitive Homogeneous And Resolved PEaks in Real time (SHARPER) enhances 31P NMR signals by collapsing the target resonance into an extremely narrow singlet and eliminating the effects of field inhomogeneity. After demonstrating the advantage of this tool in static conditions (up to 10-fold enhancement factor on SNR), the customized on-line setup has been used to monitor a faster reaction (in the order of minutes), that could not be followed with traditional 31P NMR sequences.LauraTadiello1996 -VerfasserInaut1372035028TorstenBeweries1982 -AkademischeR BetreuerIndgs1363494470000-0002-2416-8874Leibniz-Institut für Katalyse e. V.BjörnCorzilius1979 -AkademischeR BetreuerIndgs135774721Universität Rostock, Institut für Chemie38329-6Universität Rostock1419 - 19761990 -Grad-verleihende Institutiondgg2147083-2Universität Rostock. Mathematisch-Naturwissenschaftliche FakultätGrad-verleihende Institutiondgghttps://purl.uni-rostock.de/rosdok/id00004876urn:nbn:de:gbv:28-rosdok_id00004876-110.18453/rosdok_id00004876540 ChemieMathematisch-Naturwissenschaftliche Fakultätalle Rechte vorbehaltenNutzungsrechte erteiltLizenz Metadaten: CC0frei zugänglich (Open Access)en2024Universität RostockRostockmonographic202420242025Universitätsbibliothek RostockRostock2025Universitätsbibliothek Rostockhttps://purl.uni-rostock.de/rosdok/id00004876Torsten Beweries (Leibniz-Institut für Katalyse e. V.) ; Björn Corzilius (Universität Rostock, Institut für Chemie)[{"name":"Beweries, Torsten","affil":"Leibniz-Institut für Katalyse e. V."},{"name":"Corzilius, Björn","affil":"Universität Rostock, Institut für Chemie"}]Dissertation, Universität Rostock, 2024Nuclear magnetic resonancevorgelegt von Laura Tadiello Beweries, Torsten Leibniz-Institut für Katalyse e. V. Corzilius, Björn Universität Rostock, Institut für Chemie 2025-07-21T13:14:54.948Z 2025-07-21T13:40:31.721Z 2025-07-31T13:40:31.730Z editorFG {"identifier":"rosdok/id00004876","type":"local_id","additional":"","service":"MCRLocalID","created":"2025-07-21T13:14:56.468Z"} {"identifier":"urn:nbn:de:gbv:28-rosdok_id00004876-1","type":"dnbUrn","additional":"","service":"RosDokURN","created":"2025-07-21T13:14:56.519Z"} {"identifier":"https://purl.uni-rostock.de/rosdok/id00004876","type":"purl","additional":"","service":"RosDokPURL","created":"2025-07-21T13:14:56.532Z","registrationStarted":"2025-07-21T13:40:30.293Z"} {"identifier":"10.18453/rosdok_id00004876","type":"doi","additional":"","service":"RosDokDOI","created":"2025-07-21T13:14:56.543Z","registrationStarted":"2025-07-21T13:40:29.903Z","registered":"2025-07-21T13:40:31.716Z"} MCRJANITORfulltextfile/rosdok_disshab_0000003287/rosdok_derivate_0000225098/Tadiello_Dissertation_2025.pdfDevelopment of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistryDevelopment of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistrygnd:1372035028gnd:136349447orcid:0000-0002-2416-8874gnd:135774721gnd:38329-6gnd:2147083-2gnd:1372035028gnd:136349447orcid:0000-0002-2416-8874gnd:135774721gnd:38329-6gnd:2147083-2rosdok_disshab_0000003287-d598161e52gnd:1372035028Laura TadielloLaura Tadiellorosdok_disshab_0000003287-d598161e66gnd:136349447orcid:0000-0002-2416-8874Torsten BeweriesTorsten Beweriesrosdok_disshab_0000003287-d598161e83gnd:135774721Björn CorziliusBjörn Corziliusrosdok_disshab_0000003287-d598161e98gnd:38329-6Universität RostockUniversität Rostockrosdok_disshab_0000003287-d598161e112gnd:2147083-2Universität Rostock. Mathematisch-Naturwissenschaftliche FakultätUniversität Rostock. Mathematisch-Naturwissenschaftliche FakultätLaura TadielloTorsten BeweriesBjörn CorziliusUniversität RostockUniversität Rostock. Mathematisch-Naturwissenschaftliche FakultätLaura TadielloTorsten BeweriesBjörn CorziliusUniversität RostockUniversität Rostock. Mathematisch-Naturwissenschaftliche FakultätLaura TadielloRostockUniversität Rostockepub.dissertationhttps://purl.uni-rostock.de/rosdok/id00004876urn:nbn:de:gbv:28-rosdok_id00004876-110.18453/rosdok_id00004876Benchtop low-field (LF) NMR spectroscopy is a valuable tool for reaction monitoring and its application in catalysis. It is particularly attractive thanks to its low-cost and portability (i.e., the instrument can be installed right next to the fume hood). However, crucial quantitative results, e.g., kinetic profiles, cannot be correctly determined the moment degradation of an air- and moisture-sensitive catalyst occurs. Therefore, inertness of the entire setup must be guaranteed. In the first part of this thesis, it is demonstrated that this challenge could be overcome to meet the experimental requirements of highly oxygen-sensitive rhodium diphosphine complexes, relevant for homogeneous catalysis. Indeed, a commercially available benchtop LF NMR spectrometer has been evolved into an inert customized flow setup. Catalytic hydrogenation monitoring via LF 1H and 31P NMR spectroscopy proved to be suitable with this flow setup despite the relatively low concentration of the investigated species (ca. 10 mM). In the second part of the thesis, limitations due to the low magnetic field of the benchtop spectrometer (1.9 T) and the relative insensitivity of 31P compared to 1H nucleus have been faced. 31P NMR signal-to-noise ratios (SNRs) have been improved using advanced pulse sequences. Sensitive Homogeneous And Resolved PEaks in Real time (SHARPER) enhances 31P NMR signals by collapsing the target resonance into an extremely narrow singlet and eliminating the effects of field inhomogeneity. After demonstrating the advantage of this tool in static conditions (up to 10-fold enhancement factor on SNR), the customized on-line setup has been used to monitor a faster reaction (in the order of minutes), that could not be followed with traditional 31P NMR sequences.20242024Torsten Beweries (Leibniz-Institut für Katalyse e. V.) ; Björn Corzilius (Universität Rostock, Institut für Chemie)[{"name":"Beweries, Torsten","affil":"Leibniz-Institut für Katalyse e. V."},{"name":"Corzilius, Björn","affil":"Universität Rostock, Institut für Chemie"}]Dissertation, Universität Rostock, 2024Nuclear magnetic resonancevorgelegt von Laura Tadiello[xslt]Saxonrosdok/id00004876https://purl.uni-rostock.de/rosdok/id00004876193140179910.18453/rosdok_id00004876urn:nbn:de:gbv:28-rosdok_id00004876-1Laura TadielloTadiello LauraDevelopment of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistryDissertationdoctoral thesisUniversität Rostock, 2024Benchtop low-field (LF) NMR spectroscopy is a valuable tool for reaction monitoring and its application in catalysis. It is particularly attractive thanks to its low-cost and portability (i.e., the instrument can be installed right next to the fume hood). However, crucial quantitative results, e.g.,…Laura TadielloDevelopment of low-field flow 31P NMR spectroscopy for reaction monitoring in organometallic chemistryNuclear magnetic resonanceUniversitätsbibliothek Rostockhttps://purl.uni-rostock.de/rosdok/id00004876LauraTadiello1996 -VerfasserInaut1372035028TorstenBeweries1982 -AkademischeR BetreuerIndgs1363494470000-0002-2416-8874Leibniz-Institut für Katalyse e. V.BjörnCorzilius1979 -AkademischeR BetreuerIndgs135774721Universität Rostock, Institut für Chemie38329-6Universität Rostock1419 - 19761990 -Grad-verleihende Institutiondgg2147083-2Universität Rostock. Mathematisch-Naturwissenschaftliche FakultätGrad-verleihende Institutiondgg[purl]https://purl.uni-rostock.de/rosdok/id00004876[urn]urn:nbn:de:gbv:28-rosdok_id00004876-1[doi]10.18453/rosdok_id00004876open_access20242024epoch:21th_centuryrfc5646:endoctype:epub.dissertationaccesscondition:openaccessSDNB:540institution:unirostock.mnfstate:published