Proteus thermal analysis software

DSC measurements were performed with a DSC 204F1 Phoenix^® (Netzsch Gerätebau GmbH, Selb, Germany) with an integrated auto-sampler. All measurements were conducted under nitrogen atmosphere with a N₂ flow rate of 40 mL/min. For each measurement, about 20.2 ± 0.6 mg of the pre-mixed resin was weighted into aluminum crucibles (Concavus Pan And Lid From Al, Netzsch Gerätebau GmbH, Selb, Germany), which were sealed and exposed to a temperature ramp ranging from 20 to 220 °C with five heating rates (2, 5, 10, 15 and 20 °C/min). All DSC experiments were repeated three times. The changes in enthalpy were recorded and analyzed using the Proteus Thermal Analysis software (Netzsch Gerätebau GmbH, Selb, Germany). The data were exported to the Kinetics Neo Software (Netzsch -Gerätebau GmbH, Selb, Germany), with which the kinetic parameters for the Friedman (iso-conversional method) and Kamal-Sourour (model fitting method) models were obtained.
The degree of cure (α) directly correlates with the measured heat flow ( $\Delta H_t$ ) during the reaction as follows: ${\alpha }_t=\frac{\Delta H_t}{\Delta H_{Total}}$
where ${\alpha }_t$ represents the degree of cure at a specific time, $\Delta H_t$ is the overall released heat at a specific time and $\Delta H_{Total}$ corresponds to the overall released heat during the complete reaction.

Infrared measurements were made using a Fourier Transform Infrared (FTIR) spectrometer (PerkinElmer, Waltham, MA, USA) equipped with a single reflection attenuated Total Reflectance (ATR) diamond, operation in the 4000–600 cm⁻¹ mid-IR region and 32 scans/samples. All spectra were corrected for light reflectance penetration and baseline displacement.
Micro-Raman spectra were recorded at room temperature, using a Renishaw InVia Qontor spectrometer, equipped with an optical microscope. This study was performed using 633 nm of a He-Ne laser as excitation. The maximum laser power used was 100 mW, which has been found to be suitable for the measurements without heating the samples. The microscope is equipped with a 50× long working distance lens and the scattered light was registered in the 3500–100 cm⁻¹ spectral range. The spectral resolution is better than 2 cm⁻¹.
Thermal gravimetric analysis (TGA) from Netzsch (STA449) was used, equipped with a Pt/Rh crucible (diameter of 6.8 mm, volume 85 μL) with a lid. The sample was heated from 25 to 600 °C with a temperature slope of 10 K min⁻¹ in a streaming nitrogen atmosphere (purge: 50 mL min⁻¹) to suppress oxidation. The gradient and measurement started at 25 °C. An empty Pt/Rh crucible served as a reference test. Integration of the TGA peaks was performed using Proteus Thermal Analysis Software from Netzsch.

Each sample’s melting and crystallization profile was studied by using the differential scanning calorimeter (200 F3 DSC Maia, NETZSCH, Selb, Germany). The acquired thermograms were processed by using Proteus thermal analysis software (NETZSCH, Selb, Germany). The test was conducted under the nitrogen environment. Oleogel samples (~15 mg) were placed in hermetically sealed aluminum pans and a pierced lid. A properly sealed and empty aluminum pan remained as the reference sample. Thermal properties of the prepared oleogel were recorded in the temperature range from 0 to 100 °C during the heating cycle and from 100 to 0 °C during the cooling cycle. The samples were kept at isothermal conditions for 5 min: at 0 °C, before the heating cycle, and for 5 min at 100 °C, before the start of the cooling cycle. The thermal scanning rate was 5 °C/min.

Starch (3.5 mg) was loaded into an aluminum pan (Netzsch, Germany) and distilled water was added using a micropipette to create a suspension with a 75% moisture content. Samples were hermetically sealed and equilibrated for 24 h at room temperature before being heated in the DSC. The measurements were conducted at a heating rate of 10 °C/min from 20–100 °C. The enthalpy of the phase transitions (ΔH₁ J per g d.w.b. of starch) was measured from the endotherm of DSC thermograms using the Netzsch Proteus–Thermal Analysis software (Netzsch, Germany) based on the mass of the dry solids. The onset temperature (T_o1), peak temperature (T_p1), and conclusion temperature (T_c1) were calculated. The gelatinization temperature range (ΔT₁) was calculated as T_c1-T_o1. The peak height index (PHI₁) was computed from the ΔH₁/(T_p1-T_o1) ratio as described by Kaur [3 (link)]. The reported values are the means of four measurements.

Thermal properties of raw noodles were analysed using a differential scanning calorimeter (DSC; Netzsch DSC 214 Polyma) based on published methods [23 (link)]. Raw noodles were freeze-dried (Virtis SP Scientific, Warminster, PA, USA) for 48 hours and ground with a mortar and pestle. Ground samples (4–6 mg) were placed in Concavus aluminium pans (Netzsch, Germany) with 10 μL of DI water added. The pans were then hermetically sealed with lids. The analysis was carried out from 10 to 95 °C at a heating rate of 10 °C/min with an empty sealed reference pan. The parameters onset temperature (T_o), peak temperature (T_p), end temperature (T_e) and enthalpy of gelatinisation (peak area; ΔH) were analysed using the Netzsch Proteus Thermal Analysis software (Netzsch, Germany). All measurements for DSC were done in triplicates.