Colloidal and Thermal Stability of Three-Component Hybrid Materials Containing Clay Mineral, Polysaccharide and Surfactant.

The paper presents the colloidal and thermal stability of the three-component hybrid materials containing halloysite, polysaccharides (alginic acid, cationic cellulose and hydroxyethyl cellulose) and Tritons. TX-100, TX-165 and TX-405 were used as non-ionic surfactants. Stability and other properties of the hybrid materials were tested by the following methods: UV-Vis, TGA (thermogravimetric analysis) and DSC (differential scanning calorimetry), CHN (elemental analysis), SEM-EDX (scanning electron microscopy with energy dispersive X-ray spectroscopy) and tensiometry. According to the results with the increasing polymer concentration the colloidal stability of the tested systems also increases. Moreover, the addition of the surfactants causes the increase of polysaccharide adsorption but the colloidal stability of the tested systems decreases due to large weights of formed aggregates. As follows from the thermal analysis, the comparison of the TG/DTG-DSC curves obtained for the investigated polymers confirms that their thermal decomposition courses have some common features. The obtained results have the application potential in the formation of the materials for the pollutants removal from water and sewages.

Textural and Thermal Properties of the Novel Fucoidan/Nano-Oxides Hybrid Materials with Cosmetic, Pharmaceutical and Environmental Potential.

The main purpose of the research was to obtain and study hybrid materials based on three different nano-oxides commonly used in the cosmetic and pharmaceutical industries: Al2O3, TiO2, and ZnO, with the natural bioactive polysaccharide fucoidan. Since the mentioned oxides are largely utilized by industry, there is no doubt that the presented studies are important from an environmental point of view. On the basis of the textural studies (dynamic light scattering DLS, low temperature nitrogen adsorption, X-ray diffraction analysis XRD, scanning electron microscopy SEM) it was proved that the properties of the hybrid materials differ from the pure components of the system. Moreover, the advanced thermal analysis (TG-DTG-DSC) combined with the evolved gas analysis using Fourier transformed infrared spectroscopy (FTIR) and mass spectrometry were applied to describe the thermal decomposition of fucoidan, oxides and hybrid materials. It was found that the interactions between the polymer and the oxides results in the formation of the hybrid materials due to the functionalization of the nanoparticles surface, and that their thermal stability increased when compared to the pure substrates. Such findings definitely fill the literature void regarding the fucoidan based hybrid materials and help the industrial formulators in the preparation of new products.

Analysis of adsorption energy distribution in selected hydrophilic-interaction chromatography systems with amide, amine, and zwitterionic stationary phases.

Adsorption mechanisms of caffeine, quercetin, and phenol as test substances in various chromatographic systems have been analyzed. The investigations were conducted using three different chromatographic columns packed with polar bonded stationary phases, that is, amide, amine, and zwitterionic. Methanol-water and acetonitrile-water systems with different organic solvent contents have been used as mobile phases. On the basis of adsorption isotherms obtained for the tested systems, Scatchard plots and adsorption energy distributions have been determined. The most likely retention mechanisms have been discussed. The results of investigations indicate that (i) the surfaces of tested adsorbents are energetically heterogeneous, and (ii) the main role in sorption mechanism is played by low-energy sites.

Synthesis, spectroscopic characterization and biological activities of complexes of light lanthanide ions with 3-hydroxyflavone.

New solid compounds of light lanthanide ions with 3-hydroxyflavone were synthesized in good yields (up to 85 %). The resulting complexes have been thoroughly characterized using various analytical and spectral techniques, including elemental analysis, complexometry, thermogravimetry, UV-VIS, FT-IR, 1H NMR, 109AgNPET LDI MS and fluorescence spectroscopy. The molecular formulas of the complexes were determined as follows: Ln(3HF)3, where 3HF-3-hydroxyflavone, Ln = La(III), Pr(III), Nd(III) and Ln(3HF)3·nH2O, where n = 1 for Ln = Ce(III), Sm(III), Eu(III), and n = 2 for Gd(III). Thermogravimetric studies revealed that the water molecules in the hydrated compounds are located in the outer coordination sphere. Based on the spectral data, it was noted that lanthanide ions interacted with the 3OH and 4CO groups of 3-hydroxyflavone. The effect of lanthanide ion chelation on the excited-state intramolecular proton transfer (ESIPT) process and fluorescence emission of 3HF was investigated. It was found that coordination with metal ions can suppress the ESIPT process and enhance the fluorescence emission of 3HF. The synthesized compounds were also screened for their antibacterial activity, free radical scavenging capacity, and interaction with BSA. The results showed that the complexes exhibit higher biological activity compared to the ligand.

Synthesis, Spectral Characterization and Potential Fluorescent Properties of Three Lanthanide(III) Ions Complexes with Nalidixic Acid.

Three new solid lanthanide complexes with nalidixic acid (HNal) with the stoichiometry [Ln(Nal)3]·5·.5H2O (Ln = Tb, Dy and Ho) were synthesized applying the green synthesis method from the aqueous solutions without the organic solvent addition and fully characterized by the elemental analysis, XRF, complexometric titration, gravimetric analysis, molar conductivity and solubility measurements, powder X-Ray diffraction, UV-Vis and infrared (FT-IR) spectroscopies. Moreover, the luminescent properties of the Tb(III), Dy(III), and Ho(III) complexes in the solid state and in the solutions were investigated. On the basis of the detailed spectral analysis, it was concluded that the nalidixate ligands bind to the lanthanide ions by the bidentate carboxylate and carbonyl groups while water molecules belong to the outer coordination sphere. At the excitation of UV light, the complexes exhibited characteristic emission of central lanthanide ions, the intensity of which depends significantly on the excitation wavelength and/or the solvent. Thus, the application of nalidixic acid (apart from biological activity) for the synthesis of luminescent lanthanide complexes was confirmed which can find potential applications in the field of photonic devices and/or bioimaging agents.

Potassium Complexes of Quercetin-5'-Sulfonic Acid and Neutral O-Donor Ligands: Synthesis, Crystal Structure, Thermal Analysis, Spectroscopic Characterization and Physicochemical Properties.

The coordination ability of QSA- ligand towards potassium cations was investigated. Potassium complex of quercetin-5'-sulfonate of the general formula [KQSA(H2O)2]n was obtained. The [KQSA(H2O)2] (1) was a starting compound for solvothermal syntheses of acetone (2) and dimethylsulfoxide (3) complexes. For the crystalline complexes 1-3, crystals morphology was analyzed, IR and Raman spectra were registered, as well as thermal analysis for 1 was performed. Moreover, for 1 and 3, molecular structures were established. The potassium cations are coordinated by eight oxygen atoms (KO8) of a different chemical nature; coordinating groups are sulfonic, hydroxyl, and carbonyl of the QSA- anion, and neutral molecules-water (1) or DMSO (3). The detailed thermal studies of 1 confirmed that water molecules were strongly bonded in the complex structure. Moreover, it was stated that decomposition processes depended on the atmosphere used above 260 °C. The TG-FTIR-MS technique allowed the identification of gaseous products evolving during oxidative decomposition and pyrolysis of the analyzed compound: water vapor, carbon dioxide, sulfur dioxide, carbonyl sulfide, and carbon monoxide. The solubility studies showed that 1 is less soluble in ethanol than quercetin dihydrate in ethanol, acetone, and DMSO. The exception was aqueous solution, in which the complex exhibited significantly enhanced solubility compared to quercetin. Moreover, the great solubility of 1 in DMSO explained the ease of ligand exchange (water for DMSO) in [KQSA(H2O)2].