Molecular Mobility in Amorphous Polylactic Acid Studied Using 1H–13C Cross Polarization NMR


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Abstract

The 1H–13C cross polarization nuclear magnetic resonance technique was used for the study of molecular mobility in amorphous polylactic acid. The cross polarization buildup curves for methine and methyl functional groups measured at magic angle spinning rates of 4 and 10 kHz, under Hartmann–Hahn conditions determined from corresponding Hartmann–Hahn matching profiles, confirmed the presence of 1H–13C spin pairs isolated from lattice since transient oscillations were observed in the initial stages of buildup curves. The values of dipolar coupling constants derived from Fourier transforms of cross polarization buildup curves indicate the presence of rigid methine groups and two kinds of methyl functional groups which differ in mobility. This could be due to the presence of amorphous phase with chain aggregations and phase with less spatial restrictions in this material. Fitting of theoretical expressions to experimental data provided additional information on the cross polarization process in this material.

About the authors

Mária Kovaľaková

Department of Physics, Faculty of Electrical Engineering and Informatics, Technical University of Košice

Author for correspondence.
Email: maria.kovalakova@tuke.sk
ORCID iD: 0000-0002-8104-4536
Slovakia, Park Komenského 2, Košice, 04200

Oľga Fričová

Department of Physics, Faculty of Electrical Engineering and Informatics, Technical University of Košice

Email: maria.kovalakova@tuke.sk
Slovakia, Park Komenského 2, Košice, 04200

Mária Hutníková

Department of Physics, Faculty of Electrical Engineering and Informatics, Technical University of Košice

Email: maria.kovalakova@tuke.sk
Slovakia, Park Komenského 2, Košice, 04200

Dušan Olčák

Department of Physics, Faculty of Electrical Engineering and Informatics, Technical University of Košice

Email: maria.kovalakova@tuke.sk
Slovakia, Park Komenského 2, Košice, 04200

Ivan Chodák

Polymer Institute, Slovak Academy of Sciences

Email: maria.kovalakova@tuke.sk
Slovakia, Dúbravská cesta 9, Bratislava, 845 41

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