2.2.6. Thermal Analysis

The main thermal degradation parameters of biocomposites, initial degradation temperature (Tonset), and maximum mass loss rate temperature (Tmax) were studied by TGA using a TA Instrument Q500 thermogravimetric analyzer from TA INSTRUMENTS (Delaware (New Castle, DE, USA)). Then, those samples with an average weight between 8 and 10 mg were placed in standard platinum crucibles of 70 µL. In this case, biocomposites were subjected to the following temperature program: from 30 to 600 ◦C under nitrogen (N2) atmosphere at a rate of 10 ◦C/min, and from 600 to 1000 ◦C under oxygen (O2) atmosphere at a rate of 10 ◦C/min with a purge gas flow of 10 mL/min.

Later on, thermal transitions of developed biocomposites were studied by differential scanning calorimetry (DSC) in a DSC Q200 calorimeter from TA INSTRUMENTS (New Castle, DE, USA). Then, those samples with an average weight of 8–10 mg were placed in standard aluminum crucibles and subjected to a three-step program that consisted of an initial heating cycle from 0 ◦C to 250 ◦C at a rate of 10 ◦C/min to remove thermal history, followed by cooling to −20 ◦C at a rate of 5 ◦C/min, and a second heating cycle to 350 ◦C at a rate of 10 ◦C/min. All the tests were run in an N<sup>2</sup> atmosphere with a constant flow of 50 mL/min. Finally, thermal transitions were determined: temperature (Tc) and enthalpy (∆Hc) of crystallization after the cooling cycle and temperature (T<sup>f</sup> ) and enthalpy of fusion (∆H<sup>f</sup> ) after the second heating.
