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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)

  • Benchtop 1H-NMR and FTIR have both been successfully developed for size-exclusion chromatography (SEC) applications. The latest implementations of these methods by Wilhelm and collaborators[1-3] have taken advantage of commerically available low-cost equipment, and a provide a means to obtain slice-by-slice spectra for the monitoring of functional groups in polymer separations. Demonstrated applications include the detection of highly diluted chains in a polymer blend (e.g., PS/PMMA), copolymer content determination (e.g., styrene-methyl methacrylate), and butadiene isomer detection. To synthesize and characterize an end-labelled low molecular wt. poly(ethylene glycol) as a model polymer to aid in the development and validation of spectroscopic detection (FTIR and 1H-NMR) for SEC applications. A particular focus is to improve quantitation and/or detection of highly diluted funtional groups (e.g., polymer chain ends or sparsely functionalized chains) In the first approach, an isocyanateBenchtop 1H-NMR and FTIR have both been successfully developed for size-exclusion chromatography (SEC) applications. The latest implementations of these methods by Wilhelm and collaborators[1-3] have taken advantage of commerically available low-cost equipment, and a provide a means to obtain slice-by-slice spectra for the monitoring of functional groups in polymer separations. Demonstrated applications include the detection of highly diluted chains in a polymer blend (e.g., PS/PMMA), copolymer content determination (e.g., styrene-methyl methacrylate), and butadiene isomer detection. To synthesize and characterize an end-labelled low molecular wt. poly(ethylene glycol) as a model polymer to aid in the development and validation of spectroscopic detection (FTIR and 1H-NMR) for SEC applications. A particular focus is to improve quantitation and/or detection of highly diluted funtional groups (e.g., polymer chain ends or sparsely functionalized chains) In the first approach, an isocyanate with IR- and NMR-active functional groups was reacted with PEG (4000 and 10000 g/mol) to form end-functionalized chains by means of an addition reaction. The functionalization of the 10000 g/mol PEG was found to be non-homogeneous (not discussed further). The 4000 g/mol PEG was successfully functionalized to 100%, found to be homogeneous across the molecular weight distribution and could therefore serve as a model polymer for analysis by the coupled methods.zeige mehrzeige weniger

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Metadaten
Autor*innen:M. Pollack
Koautor*innen:M. Heck, M. Wilhelm, Steffen WeidnerORCiD
Dokumenttyp:Posterpräsentation
Veröffentlichungsform:Präsentation
Sprache:Englisch
Jahr der Erstveröffentlichung:2023
Organisationseinheit der BAM:6 Materialchemie
6 Materialchemie / 6.3 Strukturanalytik
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:MALDI-TOF MS; NMR; PEG; Reference materials
Themenfelder/Aktivitätsfelder der BAM:Chemie und Prozesstechnik
Veranstaltung:10th International Symposium on the Separation and Charcterization of Natural and Synthetic Macromolecules
Veranstaltungsort:Amsterdam, Netherlands
Beginndatum der Veranstaltung:01.02.2023
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:02.03.2023
Referierte Publikation:Nein
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