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13 C NMR studies of ethene‐norbornene copolymers: assignment of sequence distributions using 13 C‐enriched monomers and determination of the copolymerization parameters
Author(s) -
Wendt Ralf Alexander,
Mynott Richard,
Hauschild Klaus,
Ruchatz Dieter,
Fink Gerhard
Publication year - 1999
Publication title -
macromolecular chemistry and physics
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.57
H-Index - 112
eISSN - 1521-3935
pISSN - 1022-1352
DOI - 10.1002/(sici)1521-3935(19990601)200:6<1340::aid-macp1340>3.0.co;2-w
Subject(s) - norbornene , copolymer , triad (sociology) , metallocene , monomer , carbon 13 nmr , polymer chemistry , chemistry , nmr spectra database , post metallocene catalyst , polymerization , materials science , organic chemistry , spectral line , polymer , psychology , physics , astronomy , psychoanalysis
Ethene and norbornene were copolymerized using metallocene catalysts that produce copolymers having isolated norbornene units or microblocks with a maximum of two norbornene units. The resonances of the norbornene C 5/6 and the ethene carbon atoms, which overlap extensively in the 13 C NMR spectrum, were differentiated and assigned by comparing the 13 C NMR spectra of the copolymers obtained from monomers having 13 C at natural abundance with those prepared from feedstocks containing 13 C 1 ‐enriched ethene or 13 C 5/6 ‐enriched norbornene. The NMR analysis revealed that the chemical shifts of the norbornene C 5/6 carbon atoms are triad sensitive and those of the ethene carbon atoms are pentad sensitive. 13 C NMR analysis of copolymers containing isolated norbornene units in various proportions allowed the resonances of the norbornene C 5/6 and the ethene carbon atoms to be assigned to the respective triads and pentads. The complete triad distributions of these copolymers determined in this way were used to calculate the copolymerization parameters for a representative metallocene catalyst.