Miniflex 600

Stability of the samples in their amorphous form was monitored using a Powder X-ray Diffractometer (PXRD) Rigaku Miniflex 600 (Tokyo, Japan). Measurements were performed with a source voltage of 30 kV and 15 mA using a Cu cathode (K $\alpha$ ) as a source. Samples were measured from 5 ${}^{\circ }$ to 37 ${}^{\circ }$ with a step size of 0.05 ${}^{\circ }$ and a speed of 2 ${}^{\circ }$ /min for crystalline samples and 5 ${}^{\circ }$ /min for amorphous samples. The amorphous samples for PXRD analysis were prepared by melting crystalline samples directly on a 22 × 22 mm cover glass used as a sample holder; this procedure allowed having amorphous samples permanently mounted on the cell holder on a fixed position. Samples were stored in a desiccator at room temperature and were continuously monitored as a function of storage time.
Also, the remaining undissolved excess of the material from a tablet of a SIM–NIF 1:1 after dissolution profile was subjected to XRD analysis to investigate the possible occurrence of recrystallization during the dissolution process.

The nilotinib free base samples were promptly measured at room temperature using PXRD with two distinct types of detectors. These detectors included the semiconductor detectors equipped in the Bruker D8 and Bruker D2 powder X-ray diffractometer (Bruker in Karlsruhe, Germany), as well as the scintillation detectors equipped in the Rigaku Miniflex600 and Rigaku Smartlab powder X-ray diffractometer (Rigaku in Tokyo, Japan). The PXRD measurement parameters utilized in this study were as follows: Ag Kα radiation with a wavelength of 0.56 Å, a tube voltage of 100 kV, and a tube current of 80 mA. The scanning step size was maintained at a constant value of 0.02°, while the scanning speed was set at 6°/min, and time per step was set at 1 s. Moreover, the divergent slit was set at 0.6 mm, the anti-scatter slit was set at 3 mm. The specific PXRD diffraction angle range for the scans was set at 5–40° or 5–90°. The instrument continuously performed scans on the samples of nilotinib free base, allowing for the acquisition of PXRD patterns for each sample. In addition, it should be noted that two Rigaku Smartlab powder X-ray diffractometers were utilized in this study. These diffractometers were sourced from different universities and have been designated as Smartlab-1 and Smartlab-2 for the purposes of this research. Each sample underwent three measurements.

The dried powders were examined by powder X-ray diffraction (PXRD) using a Rigaku MiniFlex 600 X-ray diffractometer (Rigaku, Tokyo, Japan), Cu-Kα1 radiation, and Smart lab/MiniFlex guidance software version 2.0.2.1 (Rigaku, Tokyo, Japan). Gently pressed powders, after grinding, were placed in aluminum holders and analyzed at room temperature. Data were collected at a scanning rate of 3°/min, in the 2θ range of 5°–40°.