A systematic solid-state 33S NMR study of sulfur-33 enriched organosulfur compounds, e.g., diphenyl sulfide, dibenzyl sulfide, and α-S8, which are served as models for disulfide and multi-sulfide bonds in cross-linking structures in rubbers, and sulfur-33 enriched polymers is presented. High digital-resolution field-stepwise-swept solid-state NMR or zero-field solid-state NMR is introduced to overcome the spectral width problems induced by large quadrupolar interactions. Ultra-high sensitivity techniques, such as high-temperature superconducting (HTS) coils and optomechanics NMR, are developed. The present work demonstrates that, using the above combined techniques, high quality solid-state 33S NMR spectra can be obtained, yielding reliable information about 33S NMR parameters, i.e., the quadrupole coupling constant (CQ) and the quadrupole asymmetry parameter (ηQ), even if the magnitude of quadrupolar interactions is more than CQ = 45 MHz for I = 3/2. Solid-state 33S NMR becomes one of the most powerful tools for investigating the chemical properties of sulfur atoms involved in cross-linked structures in rubbers.

Development of solid-state sulfur-33 NMR for analysis of cross-linking structures in rubbers

ACS Fall 2020 Virtual Meeting

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