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Functionalized Poly(ethylene glycol)s (PEGs) as a Reference Material for Detection of Polymeric end Groups via SEC Hyphenated with FTIR and 1H-NMR (80 MHz)

  • With the online coupling (or hyphenation) of chemically-resolved spectroscopy detection with classical size-exclusion chromatography (SEC) it is possible to correlate polymer molecular size with chemical structure in a single in-situ or on-flow measurement. Medium-resolution 1H-NMR (60 MHz) spectroscopy (i.e., “desktop NMR”) and Fouriertransform Infrared Spectroscopy (FTIR) have both been developed as coupled methods (SEC-MR-NMR, SEC-FTIR) for the detection of polymer analytes by monitoring e.g. alkene or carbonyl functionality.1,2 Here, we have investigated the potential for the detection of polymer end groups, using a slightly higher field-strength spectrometer (80 MHz 1H Larmor frequency) and taking advantage of a columnless injection method that provides bulk spectra for reference. End-functionalized polymers were synthesized by reaction of PEG with toluene isocyanate, yielding ,-functionalized polymers with exactly 2 IR- and NMR-detectable functional groups per chain, as provenWith the online coupling (or hyphenation) of chemically-resolved spectroscopy detection with classical size-exclusion chromatography (SEC) it is possible to correlate polymer molecular size with chemical structure in a single in-situ or on-flow measurement. Medium-resolution 1H-NMR (60 MHz) spectroscopy (i.e., “desktop NMR”) and Fouriertransform Infrared Spectroscopy (FTIR) have both been developed as coupled methods (SEC-MR-NMR, SEC-FTIR) for the detection of polymer analytes by monitoring e.g. alkene or carbonyl functionality.1,2 Here, we have investigated the potential for the detection of polymer end groups, using a slightly higher field-strength spectrometer (80 MHz 1H Larmor frequency) and taking advantage of a columnless injection method that provides bulk spectra for reference. End-functionalized polymers were synthesized by reaction of PEG with toluene isocyanate, yielding ,-functionalized polymers with exactly 2 IR- and NMR-detectable functional groups per chain, as proven by MALD-TOF mass spectrometry. We have investigated the sensitivity (limit of detection) and spectral resolution for these functional groups in chloroform, THF, and water. Results have demonstrated a good feasibility for the simultaneous online detection of PEG backbone (M~4000 g/mol) and these end groups at the level of ca. 2 mol%.zeige mehrzeige weniger

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Metadaten
Autor*innen:M. Pollard
Koautor*innen:M. Heck, M. Wilhelm, Steffen Weidner
Dokumenttyp:Posterpräsentation
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2022
Organisationseinheit der BAM:6 Materialchemie
6 Materialchemie / 6.3 Strukturanalytik
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:MALDI-TOF MS; NMR; Polyethyleneglycol; Size exclusion chromatography
Themenfelder/Aktivitätsfelder der BAM:Chemie und Prozesstechnik
Chemie und Prozesstechnik / Chemische Charakterisierung und Spurenanalytik
Veranstaltung:33rd International Symposium on Chromatography
Veranstaltungsort:Budapest
Beginndatum der Veranstaltung:18.09.2022
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:23.12.2022
Referierte Publikation:Nein
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