New methodology to follow the evolution of squalene by-products during model compound vulcanization studies.

In this work, a new analytical methodology is proposed to separate squalene from its by-products after vulcanization, using reverse phase liquid chromatography. Regarding previous methods described in literature, the separation between reaction products and their detection have been clearly improved. A light scattering detector has been coupled to the HPLC equipment substituting the traditionally used UV detector. With these modifications is possible to detect a larger number of compounds along the reaction in only one-shot analysis. It is even possible to discern between cross-linked squalenes bonded with different sulfur chain lengths whose structures have been elucidated by mass spectrometry. Results obtained working with this methodology helped to gain more insight into the natural rubber accelerated vulcanization process.