Characterisation of the chemical structure of sulphur vulcanisates of natural rubber using 1H NMR spectroscopy


Citation

Campbell D. S., . and Chapman A. V., . and Farley P. S., . Characterisation of the chemical structure of sulphur vulcanisates of natural rubber using 1H NMR spectroscopy. pp. 155-171. ISSN 0127-7065

Abstract

1H NMR investigation of the chemical structure of crosslink sites in rubber vulcanisates has not been considered viable because of the line-broadening effects that occur even in the swollen state. A procedure is now described which produces high resolution 1H NMR spectra of polymer recovered from a natural rubber gum vulcanisate and examined in solution. The vulcanisation is specifically prepared to be free from monosulphidic crosslinks and it is disrupted under mild conditions using established thiol exchange chemistry. The spectroscopic information is interpreted in terms of characteristic protons on the carbon atoms at the sulphuration site. Conditions of sample preparation are discussed in detail as is the justification for interpretation of the data in terms of pendent thiol groups rather than pendent disulphidic groups. Spectral assignments for relevant model thiols are tabulated.


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Abstract

1H NMR investigation of the chemical structure of crosslink sites in rubber vulcanisates has not been considered viable because of the line-broadening effects that occur even in the swollen state. A procedure is now described which produces high resolution 1H NMR spectra of polymer recovered from a natural rubber gum vulcanisate and examined in solution. The vulcanisation is specifically prepared to be free from monosulphidic crosslinks and it is disrupted under mild conditions using established thiol exchange chemistry. The spectroscopic information is interpreted in terms of characteristic protons on the carbon atoms at the sulphuration site. Conditions of sample preparation are discussed in detail as is the justification for interpretation of the data in terms of pendent thiol groups rather than pendent disulphidic groups. Spectral assignments for relevant model thiols are tabulated.

Additional Metadata

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Item Type: Article
AGROVOC Term: Natural rubber
AGROVOC Term: NMR spectroscopy
AGROVOC Term: Chemical structure
AGROVOC Term: Cross-linking
AGROVOC Term: Polymers
AGROVOC Term: Vulcanization
AGROVOC Term: Thiols
AGROVOC Term: Chlorides
AGROVOC Term: Precipitation
AGROVOC Term: Rationalization
Geographical Term: Malaysia
Depositing User: Ms. Suzila Mohamad Kasim
Last Modified: 28 Apr 2025 04:31
URI: http://webagris.upm.edu.my/id/eprint/23415

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