Sta 449 f3 jupiter

The thermal stability analysis was made using a Jupiter STA 449F3 analyzer supplied by Netzsch GmbH, (Selb, Germany), which utilizes the thermogravimetry (TGA) method. The measurement involved heating a sample of an appropriate mass at the temperature range of 30–1000 °C with a step of 10 °C/min, in a nitrogen atmosphere. The analysis was performed by using the TGA-DTA attachment.

The thermal properties of the membranes were characterized by TGA (Jupiter STA 449 F3; NETZSCH, Bavaria, Germany). Prior to analysis, the samples were dried for 3 h at 105 °C in a drying oven. Measurements were recorded under a nitrogen atmosphere with a heating rate of 10 °C/min from 50 °C to 450 °C.

Coupled thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR) were conducted under nitrogen atmosphere to identify potential changes in decomposition modes that might occur due to crosslinking. TGA measurements were conducted at a heating rate of 20 K/min between 50 and 800 °C and 70 mL nitrogen flow. The onset temperature is defined as 99% residual mass. All tests were conducted three times, and averaged curves are presented. Sample weights were kept constant at 10 ± 1 mg. TGA and DSC analysis were conducted using a simultaneous scanning analysis device, STA F3 449 Jupiter, from Netzsch (Selb, Germany). FTIR gas analysis was performed simultaneously to TGA measuring using direct coupling through a 230 °C temperature-controlled transfer line. The FTIR unit was a Tensor 2 from Bruker Corp. (Billerica, MA, USA). FTIR gas-cell temperatures were controlled at 200 °C; 32 scans were averaged. The gas transfer refers to a 30 s measurement delay between the TGA and FTIR results, which corresponds to 10 °C (20 K/min).
Additionally, TGA measurements were used to calculate decomposition activation energies using the methods described by Vyazovkin [27 (link)] and Ozawa [28 (link)]. The heating rates used were 2.5, 5 and 10 K/min, under nitrogen atmosphere.

Thermogravimetric analysis (TGA) and coupled Fourier-transform infrared spectrometry (FTIR) were used to analyze changes in the decomposition behavior. TGA measurements were conducted at various heating rates of 2.5, 5, and 10 K/min under a nitrogen atmosphere, using constant temperature ramps between 50 and 800 °C. Therefore, an STA F3 449 Jupiter from Netzsch GmbH (Selb, Germany) was used. Decomposition/pyrolysis gases were transferred from the TGA exhaust to the FTIR gas cell Tensor 2 from Bruker Corp. (Billerica, MA, USA) via a coupled and temperature-controlled transfer line (230 °C). Due to the transfer time between the TGA exhaust and FTIR measurement, a signal delay between TGA and FTIR of about 30 s had to be considered. Activation energies were calculated from non-isothermal TGA measurements using a method suggested by Ozawa and Vyazovkin [36 (link),37 (link),38 (link)]. Calculations were performed using an open access calculation tool. The descriptions and download link can be found in [39 (link)].

Coupled thermogravimetric analysis (TGA) and Fourier transform infrared spectroscopy (FTIR) were conducted in a nitrogen atmosphere. A TGA STA F3 449 Jupiter from Netzsch (Selb, Germany) equipped with a high-speed furnace was used for the study. A steady heating rate of 20 K/min was used between 50 °C and 800 °C at a N2 flow rate of 70 mL/min. Due to high end temperatures, the sample carrier (TG-DSC) was equipped with aluminum oxide tilts. Sample weights were kept constant at 10 ± 1 mg (20 K/min). The onset temperature was defined as 99% residual mass. All tests were conducted three times, and averaged curves are presented. The FTIR unit Tensor 2 from Bruker Corp. (Billerica, Massachusetts, USA) was coupled by a 230 °C controlled transfer line. FTIR gas-cell temperatures were controlled at 200 °C; 32 scans were averaged. A 30 s measurement delay occurred between TGA and FTIR results, which corresponds to 10 °C.

Different types of equipment were used interchangeably to carry out the DSC and TGA experiments. A simultaneous thermal analyzer Netzsch STA 449 F3 Jupiter was used. A DSC Q100 V9.9 Build 303 (TA instruments) was used. Additionally, a TGA Q5000 V3.17 Build 265 (TA instruments) equipment was employed. The samples were placed (2–4 mg) in sealed non-hermetic aluminum pans and were scanned at a heating rate of 10 °C/min from 30−400 °C under a dry nitrogen atmosphere. The calculated glass temperature (T_g) values of synthesized solid forms were predicted employing the Gordon–Taylor equation [18 (link)].
$$\begin{gathered} {\mathrm{T}}_{\mathrm{g}\mathrm{m}\mathrm{i}\mathrm{x}}=\frac{{\mathrm{w}}_1{\mathrm{T}}_{\mathrm{g}1}+{\mathrm{w}}_2{\mathrm{T}}_{\mathrm{g}2}\mathrm{K}}{{\mathrm{w}}_1+{\mathrm{w}}_2\mathrm{K}} \\ \mathrm{K}=\frac{{\mathrm{T}}_{\mathrm{g}1}·{\mathsf{\rho }}_1}{{\mathrm{T}}_{\mathrm{g}2}·{\mathsf{\rho }}_2} \end{gathered}$$
T_g1 and T_g2 are glass transition of components 1 (FLV: 69.5 °C) [10 (link)] and 2 (PGZ·HCl: 64.4 °C) [19 (link)], w₁ and w₂ are weight fractions of the components, and T_gmix is the glass transition of the coamorphous mixture. Density values were obtained from the literature: FLV (1.20 g/cm³) [20 ] and PGZ·HCl (1.26 g/cm³) [21 ].
The crystallinity of the participating drugs within the coamorphous mixture was determined using the Rawlinson equation [22 (link)].
$$\%\mathrm{C}\mathrm{r}\mathrm{y}\mathrm{s}\mathrm{t}\mathrm{a}\mathrm{l}\mathrm{l}\mathrm{i}\mathrm{n}\mathrm{i}\mathrm{t}\mathrm{y}=\frac{\Delta {\mathrm{H}}_{\mathrm{m} \mathrm{c}\mathrm{o}\mathrm{a}\mathrm{m}\mathrm{o}\mathrm{r}\mathrm{p}\mathrm{h}\mathrm{o}\mathrm{u}\mathrm{s}}}{\Delta {\mathrm{H}}_{\mathrm{m} \mathrm{d}\mathrm{r}\mathrm{u}\mathrm{g}}·\mathrm{w}}·100$$
where ΔH_{m coamorphous} is the enthalpy of the coamorphous mixture (J/g), ΔH_{m drug} is the enthalpy of the pure drug (J/g), and w is the weight fraction of the drug in the coamorphous mixture.

Elemental composition was
determined by inductively coupled plasma mass spectrometry (ICP-MS)
(Shimadzu ICPMS-2030), and water content was estimated using thermogravimetric
analysis (TGA) (NETZSCH STA 449 F3 Jupiter) under Ar at a heating
rate of 5 °C min^–1. Scanning electron microscopy
(SEM) was carried out on a Zeiss Merlin microscope. Synchrotron X-ray
diffraction (XRD) measurements were performed on I11 beamline of the
Diamond Light Source operating with an X-ray wavelength of 0.826872
Å. The position-sensitive detector was used to collect diffraction
patterns over the temperature range 30–450 °C with a hot-air
blower. Ex situ X-ray powder diffraction measurements
of the electrode materials were performed using a Rigaku Smartlab
diffractometer (Cu Kα). All Rietveld and Pawley refinements
were carried out using the TOPAS-Academic software.²⁹