High-Temperature MAS 1D and 2D NMR for Molecular Structure Characterization of Insoluble Polymers

• Published in: Macromolecules Vol. 36; no. 3; pp. 719 - 723
• Main Authors: Thakur, Newmark, Richard A, Kuehn, Nicole T, Gregar, Travis Q
• Format: Journal Article
• Language: English
• Published: Washington, DC American Chemical Society 11.02.2003
• Subjects: Applied sciences; Exact sciences and technology; Organic polymers; Physicochemistry of polymers; Properties and characterization; Structure, morphology and analysis; High resolution; Alkyl acrylate copolymer; Insoluble compound; Molecular structure; Propylene polymer; NMR spectrometry; Experimental study; Two dimension spectrometry; Magic angle; Crosslinked copolymer; Solid state; Investigation method; Isotactic polymer; Polycaprolactone; Butyl methacrylate copolymer
• ISSN: 0024-9297; 1520-5835
• DOI: 10.1021/ma020987k

High-resolution solid-state NMR spectra can be obtained of cross-linked and high molecular weight polymeric materials by using a combination of magic-angle spinning and high temperature. The resolution of the spectra can be comparable to that seen in solution NMR spectroscopy. This enables standard solution 2D NMR pulse sequences, such as COSY, TOCSY, and HMQC, to be used to assign resonances in these systems. It has been found that short duration pulse sequences work better than long sequences. For observing heteronuclear correlations, carbon-detected 2D pulse sequences appear to have less stringent instrumental setup requirements than proton-detected 2D sequences.