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In this work, the isothermal decomposition of poly(methyl methacrylate) synthesized in bulk by the radical route of methyl methacrylate in the presence of azobisisobutyronitrile as the initiator was carried out and monitored for the first time with the DART-Tof-MS technique at different temperatures. Nuclear magnetic resonance (NMR) analysis revealed a predominantly atactic microstructure, and size-exclusion chromatography (SEC) analysis indicated a number average molecular weight of 3 × 105 g·mol−1 and a polydispersity index of 2.47 for this polymer. Non-isothermal decomposition of this polymer carried out with thermogravimetry analysis (TGA) showed that the weight loss process occurs in two steps. The first one starts at approximately 224 °C and the second at 320 °C. The isothermal decomposition of this polymer carried out and monitored with the DART-Tof-MS method revealed only one stage of weight loss in this process, which begins at approximately 250 °C, not far from that of the second step observed in the case of the non-isothermal process conducted with the TGA method. The results obtained with the MS part of this technique revealed that the isothermal decomposition of this polymer regenerates a significant part of methyl methacrylate monomer, which increases with temperature. This process involves radical chain reactions leading to homolytic chain scissions and leading to the formation of secondary and tertiary alkyl radicals, mainly regenerating methyl methacrylate monomer through an unzipping rearrangement. Although they are in the minority, other fragments, such as the isomers of 2-methyl carboxyl, 4-methyl, penta-2,4-diene and dimethyl carbate, are also among the products detected. At 200 °C, no trace of monomer was observed, which coincides with the first step of the weight loss observed in the TGA. These compounds are different to those reported by other researchers using TGA coupled with mass spectrometry in which methyl isobutyrate, traces of methyl pyruvate and 2,3-butanonedione were detected.

A series of poly(ethylene-co-vinyl alcohol)/titanium dioxide (PEVAL/TiO2) nanocomposites containing 1, 2, 3, 4 and 5 wt% TiO2 were prepared by the solvent casting method. These prepared hybrid materials were characterized by Fourier-transform infrared (FT-IR), X-ray diffraction (XRD), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). The pores and their interconnections inside these nanocomposites were created using naphthalene microparticles used as a porogen after having been extracted by sublimation under a high vacuum at temperatures slightly below the glass transition temperature. A cellular activity test of these hybrid materials was performed on human gingival fibroblast cells (HGFs) in accordance with ISO 10993-5 and ISO 10993-12 standards. The bioviability (cell viability) of HGFs was evaluated after 1, 4 and 7 days using Alamar Blue®. The results were increased cell activity throughout the different culture times and a significant increase in cell activity in all samples from Day 1 to Day 7, and all systems tested showed significantly higher cell viability than the control group on Day 7 (p < 0.002). The adhesion of HGFs to the scaffolds studied by SEM showed that HGFs were successfully cultured on all types of scaffolds.