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Multidimensional NMR studies of poly(ethylene-co-1-octene) copolymers and poly(ethylene-co-vinyl acetate-co-carbon monoxide) terpolymers

Nuamthanom, Anuttra

Abstract Details

2007, Doctor of Philosophy, University of Akron, Chemistry.

The comonomer and stereo-sequences of poly(ethylene-co-1-octene) samples with varying 1-octene content and degree of tacticity were investigated using high-temperature (120 °C) one- and two- dimensional (1D and 2D) nuclear magnetic resonance (NMR) techniques on a 750 MHz instrument. The techniques used include quantitative 13C NMR, pulsed-field-gradient (PFG) 1H -13C heteronuclear single quantum coherence(gHSQC), heteronuclear multiple bond correlation (gHMBC) and heteronuclear single quantum coherence-total correlation spectroscopy (gHSQC-TOCSY). Diffusion-ordered 2D NMR spectroscopy (DOSY) was used to confirm that the copolymer samples were not mixtures of two copolymers with different MW. Quantitative analysis of octene content was determined from quantitative 13C NMR experiments. The degree of tacticity was established by quantitative volume integration of 2D gHSQC NMR spectra.

The comonomer sequence distributions and the resonance assignments of poly(ethylene-co-vinyl acetate-co-carbon monoxide), polyEVC* terpolymer prepared from 13C-labeled carbon monoxide were also investigated using high temperature (120 °C) multidimensional (1D, 2D and 3D) NMR experiments on the same spectrometer. The NMR techniques used include 1D- 1H, 13C, 2D- gHSQC, gHMBC, gHSQC-TOCSY, 3D-gHCACX and 3D-gHCACX-HH-TOCSY NMR experiments. With 13C labeling of the polymer combined with high resolution multidimensional NMR experiments, pentad monomer sequence assignments can be made for the carbon monoxide (C)-centered pentads. The degradation of polyEVC* was also examined by 1D and 2D NMR. The NMR spectra show that α, β –unsaturated carbonyl groups are a degradation product in this terpolymer, arising from elimination of acetic acid from CV dyads.

Peter Rinaldi (Advisor)
Chrys Wesdemiotis (Other)
Matthew Espe (Other)
Daniel Smith (Other)
Scott Collins (Other)
140 p.

Recommended Citations

Citations

  • Nuamthanom, A. (2007). Multidimensional NMR studies of poly(ethylene-co-1-octene) copolymers and poly(ethylene-co-vinyl acetate-co-carbon monoxide) terpolymers [Doctoral dissertation, University of Akron]. OhioLINK Electronic Theses and Dissertations Center. http://rave.ohiolink.edu/etdc/view?acc_num=akron1183614323

    APA Style (7th edition)

  • Nuamthanom, Anuttra. Multidimensional NMR studies of poly(ethylene-co-1-octene) copolymers and poly(ethylene-co-vinyl acetate-co-carbon monoxide) terpolymers. 2007. University of Akron, Doctoral dissertation. OhioLINK Electronic Theses and Dissertations Center, http://rave.ohiolink.edu/etdc/view?acc_num=akron1183614323.

    MLA Style (8th edition)

  • Nuamthanom, Anuttra. "Multidimensional NMR studies of poly(ethylene-co-1-octene) copolymers and poly(ethylene-co-vinyl acetate-co-carbon monoxide) terpolymers." Doctoral dissertation, University of Akron, 2007. http://rave.ohiolink.edu/etdc/view?acc_num=akron1183614323

    Chicago Manual of Style (17th edition)