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SEC‐MR‐NMR: Online Coupling of Size Exclusion Chromatography and Medium Resolution NMR Spectroscopy
Author(s) -
Cudaj Markus,
Guthausen Gisela,
Hofe Thorsten,
Wilhelm Manfred
Publication year - 2011
Publication title -
macromolecular rapid communications
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.348
H-Index - 154
eISSN - 1521-3927
pISSN - 1022-1336
DOI - 10.1002/marc.201000760
Subject(s) - nuclear magnetic resonance spectroscopy , analytical chemistry (journal) , nmr spectra database , size exclusion chromatography , resolution (logic) , proton nmr , spectrometer , materials science , polymer , copolymer , chemistry , nuclear magnetic resonance , chromatography , spectral line , organic chemistry , physics , computer science , optics , astronomy , artificial intelligence , enzyme
Online coupling of size exclusion chromatography together with medium resolution nuclear magnetic resonance (SEC‐MR‐NMR) might be one solution to the problem of chemically sensitive detection in liquid polymer chromatography. By use of a combination of SEC with a table‐top, specially designed 20 MHz NMR spectrometer, based on a permanent magnet, online 1 H NMR spectra of SEC fractions can be obtained. The integration of digital filters, mechanical shims and electronic shims led to substantially improved sensitivity and chemical selectivity compared to former TD (time domain) 20 MHz instruments. 1 H NMR spectra of PMMA and PS homopolymers as well as PS‐PMMA block copolymers were of sufficient quality to enable detection and de‐formulation of unknown polymer compounds. 1 H NMR spectra of acceptable resolution and S/N ratio were collected online during the chromatography. The SEC separation online with the NMR measurements performed well and resulted in the proof of principle of the SEC‐MR‐NMR combination.