## 2 Experimental
### Differential Scanning Calorimetry (DSC)  
The calorimetric behavior of the asphaltene samples was analyzed using a DSC SETARAM 131 instrument.  
Before starting the tests on the instrument, the calibration operations were carried out using a sample of Indium with a known weight. In fact, knowing exactly the values relating to the enthalpy (\(\Delta\)H) of the melts and the exact position of the sample of Indium, it was possible to calibrate the instrument. Then, 20-30 mg of each sample was weighed in a crucible and subsequently, the container was capped and sealed by mechanical press. From a screening carried out, it was determined that the amount of sample does not affect the trend of the calorimetric curve, but acts only on the intensity of the signals. All the tests were carried out under nitrogen flow.  
Following method was used to analyze all samples:  
1. Isotherm at 25 \({}^{\circ}\)C for 20 min;
2. Heating from 25 \({}^{\circ}\)C to 250 \({}^{\circ}\)C at 20 \({}^{\circ}\)C min\({}^{-1}\);
3. Cooling from 250 \({}^{\circ}\)C to 25 \({}^{\circ}\)C at 20 \({}^{\circ}\)C min\({}^{-1}\);
4. Isotherm at 25 \({}^{\circ}\)C for 20 min;
5. Heating from 25 \({}^{\circ}\)C to 250 \({}^{\circ}\)C at 20 \({}^{\circ}\)C min\({}^{-1}\)  
Note that the first heating and cooling cycle was effectuated to ensure identical thermal history for all samples. Indeed, during the first thermal ramp, various endothermal or exothermal peaks could be observed according to the exact starting state of the sample, which is hardly controlled through a precipitation process. After a first heating, a cooling ramp of all samples at the same controlled scan rate ensures that all samples are placed in identical starting conditions. The cooling scan rate of 20 \({}^{\circ}\)C min\({}^{-1}\) was chosen in order to maximize the probability of freezing the asphaltene samples in their amorphous state. For this reason, DSC traces obtained from the second heating ramp only displayed glass temperature (Tg) transitions that can be easily compared between the samples and thus correlate to the nature of the sample. Consequently, in this work, only the calorimetric curves derived from the second thermal ramp will be shown, described and analyzed. As reported  
\begin{table}
\begin{tabular}{c c c c c} \hline  & **Label** & **Penetration Grade** & **Softening Point** & **Asphaltene** & **Asphaltene** \\  & **(0.1 mm) \(\pm\) 1** & (\({}^{\circ}\)C) \(\pm\) 0.2** & **No Age (\%)** & **after Aging (\%)** \\ \hline Bitumen 50/70 & Type 1 & 68 & 48.8 & 26.8 & 34.2 \\ Bitumen 50/70 & Type 2 & 63 & 55.0 & 30.9 & 36.9 \\ \hline \end{tabular}
\end{table}
Table 1: Information about the bitumens.  
\begin{table}
\begin{tabular}{c c c c c} \hline  & **Label** & **Type of Additive** & **Effect** & **Dosage (\%)** \\ \hline Recycling agent 1 & TPI & Poly Phosphate & Regenerator & 4 \\ Recycling agent 2 & Soy oil & Vegetable Oil & Softener & 4 \\ Recycling agent 3 & Agent 3 & Vegetable Oil + other components & Regenerator & 6 \\ Recycling agent 4 & Agent 4 & Mineral & Softener & 6 \\ \hline \end{tabular}
\end{table}
Table 2: Information about the additives.  
in literature by thermogravimetric analysis (TGA) measurements at the temperature of 250 \({}^{\circ}\)C, the asphaltenes do not show any thermal degradation phenomena [44; 45; 46].