Formation of Alginate/Chitosan Interpenetrated Networks Revealed by EPR Spectroscopy

Abstract

This study analyzes the physico-chemical properties of interpenetrated polymer networks (IPNs) and semi-IPN resulting from cross-linking chitosan with glutaraldehyde and alginate with Ca2+ cations, as a function of the order in which the cross-linking agents are added to the polymer mixture. Three physico-chemical methods were used to assess the differences between systems: rheology, IR spectroscopy, and electron paramagnetic resonance (EPR) spectroscopy. While rheology and IR spectroscopy are commonly used to characterize gel materials, EPR spectroscopy is rarely used, but has the advantage of providing local information about the dynamics of a system. The rheological parameters, which describe the global behavior of the samples, show that semi-IPN systems have a weaker gel behavior and the order of introducing the cross-linker in the polymer systems plays a role. The IR spectra of samples resulting by adding only Ca2+ or Ca2+ as the first cross-linker are similar to that of the alginate gel, while the spectra of samples in which glutaraldehyde is firstly added resemble the chitosan gel spectrum. Using spin-labeled alginate and spin-labeled chitosan, we monitored the changes occurring in the dynamic of the spin labels due to the formation of IPN and semi-IPN. The results show that the order of adding the cross-linking agents influences the dynamic of the IPN network, and that the formation of the alginate network determines the characteristics of the entire IPN system. The EPR data were correlated with the rheological parameters and IR spectra of the analyzed samples.

UV-Crosslinked Poly(N-isopropylacrylamide) Interpenetrated into Chitosan Structure with Enhancement of Mechanical Properties Implemented as Anti-Fouling Materials

“…Therefore, the gelation time needed to be identified to ensure the formation of a three-dimensional network. Several techniques, such as light scattering (LS) [12,33], beam diffraction [13], and rheology [34][35][36], have been widely used to elucidate the mechanism of material gelation and its molecular structure. In this work, the rheological technique was used to investigate the crosslinking behavior due to its direct correlation with the evolving physical and mechanical properties of the system during the crosslinking process.…”