Nc. Nielsen et al., STRATEGIES FOR STRUCTURAL AND QUANTITATIVE-ANALYSIS OF HETEROGENEOUS BLOCK-COPOLYMERS BY C-13 MAS NMR-SPECTROSCOPY, Macromolecules, 28(6), 1995, pp. 2009-2015
Strategies for structural and quantitative analysis of unknown heterog
eneous block copolymers employing solid-state C-13 magic-angle spinnin
g (MAS) NMR techniques are presented. Combinations of standard single-
pulse, cross-polarization, cross-polarization-depolarization, and SEMU
T spectral editing MAS experiments enable efficient separation, identi
fication, and quantitation of resonances from mobile as well as immobi
le phase constituents of heterogeneous polymers. The utility of these
techniques for structural and quantitative analysis of complex polymer
s is demonstrated for three block copolymers, initially of unknown str
ucture and composition. The three samples investigated here have been
identified as polypropylene/polyethylene/ethylene-propene-diene rubber
(PP/PE/EPDM), polyethylene/ethylene-propene rubber (PE/EPR), and poly
styrene/polyethylene/butadiene rubber (PS/PE/BR).