Differential Scanning Calorimetry (DSC) analyses were performed in a DSCq20 (Waters corporation, TA Instruments, Barcelona, Spain) to observe the thermal events taking place in the formulations before and after the lyophilization process. Samples of 3 mg DEX, freeze-dried DEX-lipomers (FD DEX-lipomers), and non-FD DEX-lipomers were placed in Tzero Aluminum pans and sealed with Tzero hermetic aluminum lids with a Tzero press (Water corporation, TA instruments, Barcelona, Spain). Temperature ramps were applied from 0 to 200 °C at 10 °C/min for the formulations containing sucrose and from 20 to 277 °C at 10 °C/min for the formulations without sucrose. This was because sucrose degrades at approximately 210 °C [18 (link)] and, in DSC, it is advisable to avoid degradation temperatures.
Dsc q20
Manufactured by Waters Corporation
Sourced in Spain, United States
The DSC Q20 is a differential scanning calorimeter (DSC) manufactured by Waters Corporation. It is a thermal analysis instrument that measures the heat flow associated with phase transitions and chemical reactions in materials as a function of temperature and time.
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3 protocols using dsc q20
1
Thermal Characterization of Freeze-Dried DEX-Lipomers
2
Characterization of Piezoelectric Fibrous Membrane
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The surface morphology of fibrous membrane was characterized by Field emission scanning electron microscopy (FE-SEM, Carl Zeiss, SUPRA40VP, Germany), equipped with energy dispersive electron microscopy. Multi-Purpose High-Performance X-ray Diffractometer (MPD-XRD, PANalytical, X’PERT-PRO Powder, Netherlands) was performed to check whether Al2O3 was present in the fiber. Fourier Transform infrared spectrometer was used to analyze the piezo effect increase by comparing the peaks of β phase and α phase. A hybrid- X-ray photoelectron spectrometer system (Hybrid XPS system) was performed the presence of Al2O3 was confirmed for the Binding Energy peak of Al2O3 in the fiber. Thermal Analyzer (TGA, WATERS, DSC Q20) was performed under several 5 °C/min at 50 °C–900 °C in a nitrogen atmosphere. Universal Testing Machine (UTM, MTDI Inc., UT-020E, South Korea) was performed to compare the mechanical performance of the sensor. A 1 N load cell was used and the displacement control was set to have a speed of 20 mm/min. At least three dog-bone-shaped samples were made and evaluated for each group.
3
Characterization of Surface Morphology and Mechanical Properties
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A field-emission scanning electron microscope (FE-SEM; JEOL JSM-5900) was used to analyze the surface morphologies. The phase purity and crystalline phase of the samples were characterized using X-ray diffraction (XRD) patterns through a Rigaku X-ray diffractometer with Cu-Ka radiation from 10° to 80°. The thermal behavior was investigated by differential scanning calorimetry (DSC; DSC Q20; Waters, Milford, MA, USA) operating from room temperature to 320 °C under the air atmosphere. Mechanical properties were performed by using a universal testing machine (AG-5000G; Shimadzu Co., Kyoto, Japan) under a cross-head speed of 5 mm min−1 at room temperature. In accordance with ASTM D-638, the samples were prepared in the shape of a dumbbell, and then tensile tests were conducted on at least 3~5 specimens and the average values were reported.
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