Polymorphism and its extended form, pseudopolymorphism, significantly affect the physicochemical properties, thermal stability, and potential pharmaceutical performance of biologically active compounds. Oxicams are a class of nonsteroidal anti-inflammatory drugs (NSAIDs) widely used in clinical practice; however, they are associated with a range of adverse effects. Consequently, there is ongoing interest in developing new derivatives with improved safety profiles. Moreover, owing to their structural flexibility and ability to form intramolecular hydrogen bonds and tautomeric structures, oxicam derivatives represent an interesting class of compounds exhibiting diverse solid-state behavior. In this work, a new arylpiperazine oxicam derivative was obtained as two distinct crystalline forms and characterized using spectroscopic methods (1H NMR, 13C NMR, ESI–MS, and FTIR) together with X-ray powder diffraction (XRPD). The results confirmed that the two forms differ in crystal packing and intermolecular interactions despite retaining the same molecular structure. Their thermal behavior was investigated using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). The results demonstrated that form I is the thermodynamically stable form, whereas form II is a pseudopolymorphic form incorporating ethanol molecules during crystallization. These findings provide insights into the relationship between solvation and crystal packing in novel oxicam derivatives and contribute to a better understanding of solid-state transformations in pharmaceutically relevant molecules.

Given their reactivity, excellent catalytic properties and affinity to heavy metal, CuxS particles were introduced into the matrix of carboxylic cation exchangers (CCEs) to obtain novel hybrid ion exchangers (HIXs). The study focused on the synthesis and thermal behaviour of HIXs in which commercially available, gel-type (G) and macroreticular (M) structure CCEs were used as supports for dispersed CuxS particles. Using CCEs in the Cu2+ form and a Na2S solution, under mild conditions, HIXs containing 21.3 (G) and 17.6 (M) mass

Referring to the concept of a circular economy and using optimal experimental design (OED), the research deals with optimising the conversion of industrial residue from the water de-ironing process into a red hematite pigment. The raw, chemically pretreated sludge was thermally converted into hematite under various conditions established in the optimised procedure. The products were thoroughly characterised using XRD, Raman spectroscopy, Diffuse reflectance spectroscopy, and SEM EDS to gain better insight into the process. Because of the unambiguous and quantitative definition of colour and its individual perception, resulting in difficulty in determining the appropriate system response in the optimisation procedure, products’ quantitative colour parameters, determined in the CIELab colour space, were compared to those obtained for the commercial red hematite pigment, and the most suitable ones (a*, C*, and L*) were chosen as system responses in the optimising procedure. As a result, the optimal ranges of the process parameters—temperature and holding time—that can ensure a pigment with the desired colour were established by OED methodology. Moreover, it was found that the key factor enabling effective conversion of the studied residue into red pigment is a proper chemical pretreatment in which the process temperature is decreased to below the hematite sintering temperature.

New hybrid cation exchangers containing Cu x S clusters. Sulfidation product depends on the type of HIX and precursor. Copper and sulfur are distributed throughout the entire volume of the HIXs. High thermal stability of of prepared HIXs.

The successful development of an amorphous form of a drug demands the use of process conditions and materials that reduce their thermodynamic instability. For the first time, we have prepared amorphous ibrutinib using the quench-cooling method with very high process efficiency. In the presented study, different formulations of amorphous active pharmaceutical ingredient (API) with Soluplus (SOL) in various weight ratios 1:9, 3:7, and 1:1 were prepared. The obtained samples were stored under long-term (25 ± 2 °C/60%RH ± 5% RH, 12 months) and accelerated (40 ± 2 °C/75%RH ± 5% RH, 6 months) storage conditions. The physical stability of amorphous ibrutinib and ibrutinib–Soluplus formulations was analyzed using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), powder X-ray diffraction analysis (XRPD), Fourier transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM). The lack of significant interactions between the ingredients of the formulation was confirmed by FTIR analysis. An increase in moisture content with an increasing SOL weight ratio was observed under accelerated aging and long-term conditions. Additionally, a slight increase in the moisture content of the stored sample compared to that at the initial time was observed. The results revealed the physical strength of the polymeric systems in the presence of high humidity and temperature. The observed high thermal stability allows the use of various technological processes without the risk of thermal degradation.

In order to systematize and expand knowledge about copper-containing composite materials as hybrid ion exchangers, in this study, fine metallic copper particles were dispersed within the matrix of a carboxyl cation exchanger (CCE) with a macroporous and gel-type structure thanks to the reduction of Cu2O particles precipitated within the matrix earlier. It was possible to introduce as much as 22.0 wt% Cu0 into a gel-type polymeric carrier (G/H#Cu) when an ascorbic acid solution was used to act as a reducer of Cu2O and a reagent transforming the functional groups from Na+ into the H+ form. The extremely high shrinkage of the porous skeleton containing –COOH groups (in a wet and also dry state) and its limited affinity for water protected the copper from oxidation without the use of special conditions. When macroporous CCE was used as a host material, the composite material (M/H#Cu) contained 18.5 wt% Cu, and copper particles were identified inside the resin beads, but not on their surface where Cu2+ ions appeared during drying. Thermal analysis in an air atmosphere and under N2 showed that dispersing metallic copper within the resin matrix accelerated its decomposition in both media, whereby M/H#Cu decomposed faster than G/H#Cu. It was found that G/H#Cu contained 6.0% bounded water, less than M/H#Cu (7.5%), and that the solid residue after combustion of G/H#Cu and M/H#Cu was CuO (26.28% and 22.80%), while after pyrolysis the solid residue (39.35% and 26.23%) was a mixture of carbon (50%) and metallic copper (50%). The presented composite materials thanks to the antimicrobial, catalytic, reducing, deoxygenating and hydrophobic properties of metallic copper can be used for point-of-use and column water/wastewater treatment systems.

Due to the versality, surface imperfections and diverse redox chemistry of CuxS, hybrid ion exchangers (HIXs) containing these particles are an interesting object of research, including thermal transformation. The composite materials used for testing were strongly basic anion exchangers, with macroreticular (M) and gel-type structure (G), containing in the poly (styrene/divinylbenzene) skeleton fine particles of covellite/brochantite (M1), covellite (M2), covellite/digenite/djurleite (G1) and covellite/digenite (G2). The prepared HIXs contained 12–16 mass

In this study the interaction of polymeric support with carboxylic groups and dispersed cuprous oxide particles on thermal and wetting properties of composite materials was investigated. Carboxylic cation exchangers (CCEs) in the Cu2+ form (macroporous, M and gel-type structure, G) was reacted with an ascorbic acid/NaOH solution to obtain hybrid ion exchangers containing Cu2O fine particles (over 20.0 wt% of Cu). The results of thermal analysis, under air and under N-2, of CCEs with carboxylic groups in the H+ and Na+ form and obtained composites (M/H, M/Na, M/Na#Cu2O, M/H#Cu2O and G/H, G/Na, G/Na#Cu2O, G/H#Cu2O) were discussed. The TG/DTG curves shoved varied content of the hygroscopic water in examined materials, in the range of 4.05-22.55 wt%. It was found that similarly to M/Na and G/Na, M/Na#Cu2O and G/Na#Cu2O were stable until up to 450 degrees C, while M/H#Cu2O, G/H#Cu2O decomposed faster than M/H and G/H, below 200 degrees C. By X-ray diffraction and FTIR spectroscopy, Na2CO3, CuO, Cu2O and Cu-0 were identified in the solid residues, whose mass reached 55.0 wt%. The obtained multifunctional, thermal stable and exceptionally rich in Cu2O composite materials are potential catalysts, sorbents and biocides.

As copper and its compounds are of fundamental importance for the development of innovative materials, the synthesis of composites intended for water purification was undertaken in which submicron copper containing particles were dispersed within the matrix of a strongly basic anion exchanger, with a macroporous and gel-like structure. Due to their trimethylammonium functional groups, the host materials alone exhibited an affinity to anionic water contaminants and antimicrobial properties. The introduction of such particles as CuO, Cu2O, metallic Cu, CuO/FeO(OH), Cu4O3, Cu(OH)2, Cu4(OH)6SO4, Cu2(OH)3Cl increased these properties and demonstrated new properties. The composites were obtained unconventionally, in ambient conditions, using eco-friendly reagents. Alternative synthesis methods were compared and optimized, as a result of which a new group of hybrid ion exchangers was created (HIXs) containing 3.5–12.5 wt% of Cu. As the arrangement of the inorganic phase in the resin matrix was atypical, i.e., close to the surface of the beads, the obtained HIXs exhibited excellent kinetic properties in the process of oxidation and adsorption of As(III), as well as catalytic properties for the synthesis of triazoles via click reaction, and also antimicrobial properties in relation to Gram-positive Enterococcus faecalis and Gram-negative Pseudomonas aeruginosa and Escherichia coli, preventing biofilm formation. Using thermogravimetry, the effect of the inorganic phase on decomposition of the polymeric phase was evaluated for the first time and comprehensively, confirming the relationship and finding numerous regularities. It was also found that, depending on the oxidation state (CuO, Cu2O, Cu), copper-containing particles affected the textural properties of the polymeric phase endowing a tighter structure, limiting the porosity and reducing the affinity for water.

The thermal decomposition and kinetic parameters of four polymers, PN-1, PN-05, PN-01, and PN-005, were determined by thermogravimetry (TGA/DTG) under non-isothermal conditions. N-isopropylacrylamide (NIPA)-based polymers were synthesized by the surfactant-free precipitation polymerization (SFPP) with different concentrations of the anionic initiator potassium persulphate (KPS). Thermogravimetric experiments were carried out in the temperature range of 25–700 °C at four heating rates, 5, 10, 15, and 20 °C min−1, under a nitrogen atmosphere. Poly NIPA (PNIPA) showed three stages of mass loss during the degradation process. The thermal stability of the test material was determined. Activation energy values were estimated using Ozawa, Kissinger, Flynn–Wall–Ozawa (FWO), Kissinger–Akahira–Sunose (KAS), and Friedman (FD) methods.

Freeze drying and spray drying techniques were evaluated for encapsulation of pure hesperidin and hesperidin from citrus peel extract in Maltodextrin and Gum Arabic in order to improve hesperidin stability and solubility. Physicochemical and structural properties of the microcapsules were determined and compared with the standardized high-purity hesperidin. Solubility of obtained microcapsules, defined by high WAI (0.202-0.697 g/g), WSI (88.02-99.746 %) and OAI (2.174-4.56 g/g), caused mainly by the amorphization of hesperidin structure was significantly improved. It was also confirmed with PXRD analyses. Microcapsules were of light colour, characterized by colour changes in the range from 12.57 to 47.49 and high whiteness index (64.12-94.45). The beneficial effect of encapsulation techniques is evident in flow properties where the Hausner ratio was in the range of 1.023-1.304 and Carr's index in the range of 2.26-23.273 %. Obtained microcapsules had satisfying hesperidin retention with encapsulation efficiency from 7.56 to 65.29 % and thermal stability above 110 degrees C. The best results were obtained for pure hesperidin encapsulated with freeze drying, satisfying results were obtained for citrus peel extract encapsulated in maltodextrin using spray drying. Obtained results indicate that the encapsulation of hesperidin can protect its bioactivities from environmental conditions and improve its solubility and flow properties, hence increasing its functional capabilities as pharmaceutical and cosmetic ingredients or additives.

The effect of a cupric deposit (Cu2+, CuO) on the thermal decomposition of carboxylic cation exchangers (CCEs) is not known, and such studies may have practical significance. CCEs have a very high ion exchange capacity, so an exceptionally large amount of CuO (which is a catalyst) can be precipitated inside them. Two CCEs, macroreticular (Amberlite IRC50) and gel-like (Amberlite IRC86), served as a polymeric support to obtain copper-rich hybrid ion exchangers. Composites with CuO particles inside a polyacrylic matrix (up to 35.0 wt% Cu) were obtained. Thermal analyses under air and under N2 were performed for CCEs in the H+ and Cu2+ form with and without a CuO deposit. The results of sixteen experiments are discussed based on the TG/DTG curves and XRD patterns of the solid residues. Under air, the cupric deposit shifted the particular transformations and the ultimate polymeric matter decomposition (combustion) toward lower temperatures (even about 100–150 °C). Under N2, the reduction of the cupric deposit to metallic copper took place. Unique composite materials enriched in carbonaceous matter were obtained, as the products of polymeric matrix decomposition (free radicals and hydrogen) created an additional amount of carbon char due to the utilization of a certain amount of hydrogen to reduce Cu (II) to Cu0.

Hybrid ion exchangers (HIXs) containing fine Cu2O and Cu0 particles were subjected to thermal analysis in order to determine their hygroscopic water content (with regard to their anomalously low porosity) and to determine the effect of the oxidation state of the copper atom in the deposit on the thermal properties of composite materials. Commercially available anion exchangers, Amberlite IRA 900Cl (macroreticular, M) and Amberlite IRA 402OH (gel-like, G), were used as supporting materials. M/Cu2O, G/Cu2O, M/Cu and G/Cu, containing 4.3–8.4 wt% Cu, were subjected to thermal analysis under respectively air and N2. TG/DTG curves revealed that dry M/Cu and G/Cu contained as little as 7.2% and 4.3% hygroscopic water, while M/Cu2O and G/Cu2O contained respectively 10.6% and 9.4% (Cu0 was a stronger water repellent than Cu2O). The oxidation state of the copper atom in the deposit was found to affect the amount of the forming char, and also Cu0 was found to contribute to the formation of more char than in the pyrolysis of the pure resin (the anion exchanger with no copper deposit). Under air the two kinds of particles transformed into CuO, while under N2 metallic copper and char (from the resin phase) made up the solid residue. This means that in the pyrolysis of the HIXs the inorganic phase participated in char formation and it also transformed itself (undergoing reduction when possible). The above findings provide a basis for in-depth research aimed at the innovative use of copper-containing HIXs and at obtaining usable composite materials with a designed (organic-inorganic) composition.

The effect of the inorganic deposit on the thermal decomposition of hybrid ion exchangers (HIXs) has not been comprehensively studied before. Therefore, as part of this research anion exchangers containing cupric compound in their matrix (CuO, Cu(OH)(2) and Cm-4(OH)(6)SO4) were subjected to thermal analysis. Strongly basic commercial anion exchangers, i.e. a macroreticular anion exchanger (M) and a gel-like anion exchanger (G), were used as the host materials. M, M/CuO, M/Cu(OH)(2) and G, G/CuO, G/Cm-4(OH)(6)SO4 were subjected to thermal analysis under respectively air and N-2. The samples of the HIXs contained 57.8-84.5 mg Cu/g. The results of twelve experiments are discussed on the basis of the TG/DTG curves and XRD patterns for the solid residues. The effects of: (a) the process conditions, (b) the type of deposit and (c) the structure of the anion exchanger on the course of the thermal transformations, the process end temperature, the amount of carbonizate in the post-pyrolysis residue and the composition of the inorganic phase (CuO after combustion, Cu-0 or Cu2S after pyrolysis) were determined. It was demonstrated that during the thermal decomposition of the HIXs under N-2 the reduction of Cu(II) was taking place, and owing to this hydrogen-consuming conversion more carbonizate formed than in the pyrolysis of the pure resins, as under hydrogen deficit the hydrocarbon radicals condensed into large non-volatile particles.

The proposed study examined the characterization and stability of solid-state amorphous imatinib mesylate (IM) after 15 months under controlled relative humidity (60 ± 5%) and temperature (25 ± 2 °C) conditions. After 2 weeks, and 1, 3, 6, and 15 months, the samples were characterized using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), X-ray powder diffractometry (XRPD), attenuated total reflectance-Fourier transform infrared spectroscopy (ATR-FTIR) and scanning electron microscopy (SEM). Additionally, the amorphous form of imatinib mesylate was obtained via supercooling of the melt in a DSC apparatus, and aged at various temperatures (3, 15, 25 and 30 °C) and time periods (1–16 h). Glass transition and enthalpy relaxation were used to calculate molecular-relaxation-time parameters. The Kohlrausch–Williams–Watts (KWW) equation was applied to fit the experimental enthalpy-relaxation data. The mean molecular-relaxation-time constant (τ) increased with decreasing ageing temperature. The results showed a high stability of amorphous imatinib mesylate adequate to enable its use in solid dosage form.

The present study evaluates the effect of the cationic initiator on the hydrodynamic diameter of copolymers of N-isopropylacrylamide nanogels synthesized via a surfactant-free precipitation polymerization at 70 °C in the presence of the cationic initiator 2,2'-azobis[2- methylpropionamidine] dihydrochloride. Three types of polymeric nanoparticles were synthesized using N, N'-methylenebisacrylamide as a crosslinker. The first batch was used as a reference. The second type of particles included a poly(ethylene glycol) methyl ether-acrylate monomer, while the third type used an N-tert-butylacrylamide comonomer. The hydrodynamic diameters of the synthesized particles were between 160 and 970 nm at 18 °C. The chemical composition and morphology of the synthesized co-polymeric nanoparticles were confirmed using infrared spectroscopy, nuclear magnetic resonance and scanning electron microscopy. The zeta potentials measured via dynamic light scattering were 20.0, 17.0, -0.1 mV for the three types, respectively. The volume phase transition temperature was between 22 and 41 °C. The polydispersity index of particles synthesized with N-tert-butylacrylamide varied depending on the measurement temperature.

The chlorination process of anhydrous indium(III) oxalate with carbon tetrachloride vapour in an argon stream was studied at different temperatures (200, 250, 300, 350, 400 and 450 degrees C) and times (5, 10, 15, 20 and 25 h) each. The reaction products were analysed by determination of indium and chlorine content aimed at their purity control. From the results obtained, a new simple method was developed for preparation of pure anhydrous indium(III) chloride.

This study focused on the thermal analysis of a hybrid ion exchanger (HIX) containing 23.0 wt% hydrated ferric oxides (HFO), in which a commercially available strongly basic macroreticular anion exchanger (An) was used as the supporting material. The freeze dried An/HFO and thermally dried An/HFO were analysed (under air and under nitrogen) using TG/DTG techniques to clarify the role of HFO in the decomposition processes. The TG/DTG curves for the differently dried An/HFO differed in their shape. Freeze drying was found to be a useful method of preparing HIX for thermal analysis, considering that it prevents anion exchanger shrinkage and pore blocking. When the thermal decomposition of the host material (An) was conducted more conversions, under both air (four steps) and nitrogen (three steps), were registered than in the previous studies by other authors. The decomposition of the anion exchanger in air was found to end at the temperature of 625 degrees C, while in nitrogen it ended at 450 degrees C. The presence of HFO in the anion exchanger was found to clearly affect its decomposition in air the decomposition ended at a temperature about 75 degrees C lower, while in nitrogen it ended at a temperature about 50 degrees C higher than in the case of the anion exchanger without the deposit under the above atmospheres. The results presented in this paper shed new light on the course of the thermal analysis of anion exchangers, indicate the possibility of an unconventional way of drying HIXs to be analysed by thermogravimetry, and show that thermal processes can be used to transform spent HIXs into new alternative sorption materials containing a considerable amount of iron oxides.