TGA measurements were performed on 10–15 mg of sample, using a TA Instruments TGA Q500 apparatus (New Castle, DE, USA) at a heating rate of 10 °C/min, up to 580 °C, under nitrogen (90 mL/min). The thermal decomposition temperatures Tdonset and Tdmax stand for the temperature corresponding to the onset of the degradation and to the maximum to the derived curve, respectively.
Tga q500 apparatus
Manufactured by TA Instruments
Sourced in United States
The TGA Q500 apparatus is a thermal gravimetric analyzer used to measure the change in weight of a sample as a function of temperature or time. The instrument can be used to analyze a wide range of materials, including polymers, composites, and inorganic compounds. The TGA Q500 provides accurate and precise data on the thermal stability, decomposition, and composition of samples.
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5 protocols using tga q500 apparatus
1
Thermal Degradation Analysis
2
Thermal Stability and Glass Transition of Polymers
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Thermogravimetric analysis
(TGA) was performed using TA Instruments TGA Q500 apparatus to determine
the thermal stability of the polymers under a N2 atmosphere.
The temperature was increased to 600 °C at a heating rate of
10 °C min–1. The thermal decomposition temperature
(Td,95) was determined at 5% weight loss.
Differential scanning calorimetry (DSC) analysis was carried out
using a TA Instruments DSC Q2000 differential scanning calorimeter.
Dried samples were transferred to aluminum pans, which were hermetically
sealed. The linear polymethacrylate and de-crosslinked polymer samples
were first heated to 140–200 °C, then cooled to −50
°C, and finally heated to 140–200 °C. The (re-)crosslinked
polymer samples were first heated to 160–200 °C, then
cooled to −50 °C, and finally heated to 160–200
°C. The upper temperature limit depended on the Td,95 of the particular polymer under measurement. The
scan rate in all cases was 10 °C min–1 during
the temperature program. The Tg values
of the polymers were evaluated from the second heating scans by identifying
the inflection points.
(TGA) was performed using TA Instruments TGA Q500 apparatus to determine
the thermal stability of the polymers under a N2 atmosphere.
The temperature was increased to 600 °C at a heating rate of
10 °C min–1. The thermal decomposition temperature
(Td,95) was determined at 5% weight loss.
Differential scanning calorimetry (DSC) analysis was carried out
using a TA Instruments DSC Q2000 differential scanning calorimeter.
Dried samples were transferred to aluminum pans, which were hermetically
sealed. The linear polymethacrylate and de-crosslinked polymer samples
were first heated to 140–200 °C, then cooled to −50
°C, and finally heated to 140–200 °C. The (re-)crosslinked
polymer samples were first heated to 160–200 °C, then
cooled to −50 °C, and finally heated to 160–200
°C. The upper temperature limit depended on the Td,95 of the particular polymer under measurement. The
scan rate in all cases was 10 °C min–1 during
the temperature program. The Tg values
of the polymers were evaluated from the second heating scans by identifying
the inflection points.
3
Multimodal Materials Characterization
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Scanning electron microscopy (SEM) was performed using a JSM-IT500HR instrument (JEOL, Tokyo, Japan) in high-vacuum mode operated at an accelerating voltage of 5 kV and a probe current of 35 A. X-ray photoelectron spectroscopy (XPS) measurements were performed with an Al Kα X-ray source using a K-Alpha+ spectrometer (ThermoFisher scientific, Waltham, MA, USA). Attenuated total reflection-Fourier transform infrared spectroscopy (ATR-FTIR) was performed using a Nicolet iS50 FT-IR (ThermoFisher scientific, Waltham, MA, USA) with the range from 3800–400 cm−1. Thermogravimetric analysis (TGA) was performed using a TGA Q500 apparatus (TA Instruments, New Castle, DE, USA) under a nitrogen atmosphere at a flow rate of 100 cm3/min. Additionally, TGA was performed in the air. The temperature range was from 25 to 800 °C with a heating rate of 10 °C/min.
4
Thermogravimetric Analysis of Simvastatin Loading
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Thermogravimetric measurements (samples of ~1–4 mg) were completed from 22.5 °C to 550 °C, at a heating rate of 5 °C min−1, using a TGA Q500 apparatus (TA Instruments Inc., Guyancourt, France), under a highly-pure nitrogen atmosphere (sample purge flow rate of 60 mL min−1). The temperature and mass reading were calibrated using the Curie point of the nickel standard and using equibalance tare weights (provided by TA Instruments Inc), respectively.
The drug loading (w/w) percentage was calculated according to Equation (1).
The filling degree (v/v) was estimated according to Equation (2), taking into account the loading percentage determined by thermogravimetry (Equation (1)) the total pore volume and density of crystalline simvastatin (1.172 g cm−3 [44 (link)]).
The drug loading (w/w) percentage was calculated according to Equation (1).
The filling degree (v/v) was estimated according to Equation (2), taking into account the loading percentage determined by thermogravimetry (Equation (1)) the total pore volume and density of crystalline simvastatin (1.172 g cm−3 [44 (link)]).
5
Synthesis and Characterization of H-PMEA Copolymer
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PMEA was prepared by free radical polymerization. The polymerization was conducted in 1,4dioxane at 75 C for 6 hours making use of AIBN as the initiator. [27] [28] The polymer was precipitated from THF/hexane mixture, and dried in vacuo at 60 C for several days. The functional 2-{3-(6-methyl-4-oxo-1,4-dihydropyrimidin-2-yl)ureido}ethyl methacrylate and its Hbonding copolymer with MEA (H-PMEA) were synthesized and analyzed as reported in the literature. 29 H-PMEA copolymer prepared in this work contains 6 mol% of the functional monomer according to 1 H NMR spectroscopy (Figure S1). The molecular weight characteristics of both polymers are presented in Table 1. Differential scanning calorimetry (DSC) measurement was conducted in the temperature range of -100-50 °C and at the rate of 5.0 °C/min on a Seiko Instruments Inc. X-DSC7000 purged with N 2 . T g was determined from the second heating curve automatically, and is reported as the onset of the thermal transition. A TGA Q500 apparatus from TA Instruments was utilized to conduct thermogravimetric analyses (TGA). Samples were heated from 20 to 550 C with a heating rate of 5 C/min under either air or nitrogen flow.
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