2.2.7. Powder X-ray Diffraction (PXRD)

PXRD patterns were obtained with a laboratory X'PERT PRO MPD (PANalytical, Almelo, Netherlands) diffractometer with CuKα (λ= 1.542 Å) radiation. The generator was operated at an excitation voltage of 45 kV and anodic current of 40 mA. The following scan parameters were utilized: scan type—gonio, measurement range of 2–40◦ 2θ, step size of 0.02◦ 2θ and the time per step was 200 s. The samples were placed on a zero-background silica sample holder. Alternatively, PXRD measurements were performed using a Rigaku Miniflex II, desktop X-ray diffractometer (Tokyo, Japan) equipped with a CuKα (λ = 1.54 Å) radiation X-ray source. Dried samples were mounted on a low-background silicon sample holder and scanned over a 2θ range of 2–40 degrees [23].
