Broadband dielectric spectroscopy is applied to investigate the electrical properties of disordered perovskite-like ceramics in a wide temperature range. From the x-ray diffraction analysis it was found that the newly obtained (Na0.75Bi0.25) (Mn0.25Nb0.75)O3 ceramics consist of two chemically different phases. The major perovskite one has an orthorhombic structure described by the Pbcm space group (No 57, in yxz setting). The minor phase shows an orthorhombic symmetry, all-face-centred lattice F, with the lattice parameters a = 10.797(4) Å, b = 7.601(3) Å and c = 7.691(3) Å. The electric modulus M* formalism used in the analysis enabled us to distinguish and separate the relaxation processes, dominated by marked conductivity in the ε*(ω) representation. In the ceramics studied, the relaxation times are thermally activated and the dipole process has a clearly non-Debye behaviour. The relaxation process described with the use of the activation energy of approximately 0.4 eV and the characteristic relaxation time, τ0 = 1 × 10−11 s, was found to be related to oxygen vacancies. The low frequency relaxation shows Debye behaviour with a slightly lower activation energy and a longer characteristic time.

Purpose To investigate the effect of cryogrinding on chemical stability of the diuretic agent furosemide and its mixtures with selected excipients. Methods Furosemide was ground at liquid nitrogen temperature for 30, 60, 120 and 180 min. Mixtures of furosemide-PVP and furosemide-inulin (1:1) were milled under cryogenic conditions. Materials were analyzed by XRD, UPLC, MS and NMR.

This study for the first time investigates physicochemical properties of amorphous indapamide drug (IND), which is a known diuretic agent commonly used in the treatment of hypertension. The solid-state properties of the vitrified, cryomilled and ball-milled IND samples were analyzed using X-ray powder diffraction (XRD), mass spectrometry, nuclear magnetic resonance (NMR), infrared spectroscopy (FT-IR), differential scanning calorimetry (DSC) and broadband dielectric spectroscopy (BDS). These analytical techniques enabled us (i) to confirm the purity of obtained amorphous samples, (ii) to describe the molecular mobility of IND in the liquid and glassy state, (iii) to determine the parameters describing the liquid-glass transition i.e. Tg and dynamic fragility, (iv) to test the chemical stability of amorphous IND in various temperature conditions and finally (v) to confirm the long-term physical stability of the amorphous samples. These studies were supplemented by density functional theory (DFT) calculations and apparent solubility studies of the amorphous IND in 0.1 M HCl, phosphate buffer (pH=6.8), and water (25 and 37 °C).