Dsc 60a

All resin samples were freeze-dried, and then milled to 200 mesh particle size for analysis by FT-IR and liquid-state ¹³C-NMR spectroscopies (Bruker Biospin, Bern, Switzerland). FT-IR analysis of PF, ALPF, and DLPF samples were collected as described above. Samples of resins (50 mg) were dissolved in DMSO-d6 for liquid-state ¹³C-NMR analysis using an AVANCE III HD 600MHz spectrometer; all spectra were recorded at room temperature with a relaxation delay of 8 s over 800 scans.
DSC analysis of PF, ALPF, and DLPF resins were determined using a DSC 60A (Shimadzu Corporation, Tokyo, Japan). A 5–10 mg sample was added to an aluminum sample pan and heated at a rate of 10 °C/min from ambient temperature to 150 °C under N₂ atmosphere at a flow rate of 40 mL/min.
Thermal gravimetric analysis (TGA) was performed on a TA-60H (Shimadzu Corporation, Tokyo, Japan) under N₂ atmosphere over a temperature range of 25−800 °C, a heating rate of 10 °C/min, and a flow rate of 40 mL/min.
The gel time of phenolic resins was determined according to the Chinese National Standard (GB/T 14074.3-2006). A 5 g sample of the resin was placed in a test tube and maintained in an oil bath at 130 °C. Next, a thin wire spring was used to manually mix the sample until gelation occurred.

The physical state of the E-latex inside the NPs was characterized by the analysis of the DSC curves. The curves were obtained in a DSC cell (Shimadzu^® model DSC-60A) using aluminum crucibles with about 3.0 mg of samples, which were subsequently sealed with a press. The analyses were performed under a dynamic nitrogen atmosphere at 20 mL×min^-1 and heating rate of 5.0°C×min^-1, in the temperature range of 35 to 400°C. The DSC equipment was pre-calibrated with metal indium (purity above 99.99%, melting temperature = 156.4°C). The data obtained from the thermal events of the samples were identified in the curves obtained by the software TA-60WS^®.

Differential scanning calorimetry (DSC) analyses were performed using a SHIMADZU differential scanning calorimeter DSC-60A (SHIMADZU, Columbia, SC, USA.) thermal analyzer in a nitrogen dynamic atmosphere with a flow rate of 50 mL. min⁻¹ at a heating rate of 10 °C min⁻¹ over the range of 25–300 °C; for DSC analyses, 3.0 mg of sample was evaluated in a closed aluminum cell. Thermogravimetric (TG) analyses were performed using a NETZSCH STA 409 PC/PG (Netzsch-Gerätebau GmbH, Selb, Germany) in a nitrogen dynamic atmosphere with a flow rate of 60 mL min⁻¹ and a heating rate of 10 °C min⁻¹ over the range of 30–300 °C; for TG analyses, 6 mg of sample was evaluated in an aluminum cell. An empty aluminum cell was used as a reference for both analyses.

The thermal properties of CA-co-GLC, as well as CA were studied using the DSC method with a Shimadzu DSC 60A (Shimadzu, Kyoto, Japan) device previously calibrated with indium. Between 8 and 10 mg of film (copolymer) or powder (CA) samples were packed in aluminum pans and placed in the DSC cell. The samples were scanned from 25 to 200 °C under a nitrogen atmosphere at a heating rate of 20 °C·min⁻¹. The thermal curves obtained showed that the samples did not undergo degradation during the heating process.
The glass transition temperature, Tg, was accurately determined on the thermograms from the midpoint indicating the variation in the heat capacity versus temperature. To remove any traces of volatile compounds incrusted in the polymer matrix, such as solvent, water, and residual monomer, Tg values were taken from the second cycle of the DSC process.

NMR spectra were recorded on a Bruker 400 MHz spectrometer in CDCl₃ with tetramethylsilane (TMS) as the interval standard. Matrix Assisted Laser Desorption Ionization (coupled to a Time-Of-Flight analyzer) experiments (MALDI-TOF) was recorded on a Shimadzu GCMS 2010 PLUS. Thermogravimetric analyses (TGA) measurements were conducted by a Shimadzu DTG-60H under a heating rate of 10^oC min^–1 and a nitrogen flow rate of 50 cm³ min^–1. Differential scanning calorimetry (DSC) measurements were performed using a Shimadzu Instruments DSC-60A and DSC data were collected from 30 to 200 ^oC at a rate of 10 ^oC min^–1 under N₂ flow.

The DSC analysis of the PHEMMA, pure LIG, and PHEMMA/LIG systems and their components was performed on a Shimadzu DSC 60A (Shimadzu, Kyoto, Japan, previously calibrated with indium. Samples weighing between 8 and 10 mg were packed into aluminum DSC pans before being placed in the DSC cell. The samples were scanned from 30 to 200 °C under nitrogen atmosphere at a heating rate of 20 °C·min⁻¹. The obtained thermograms revealed that the PHEMMA/LIG system and their pure components did not undergo degradation. Glass transition temperatures T_g were derived accurately from the thermograms as the midpoint in the heat capacity variation with temperature. To eliminate all eventual volatile compounds incrusted in the polymer, such as the solvent and residual monomer, the T_g values were taken from the second run of the DSC process.