Conformational isomers of the [(5‐methyl‐2‐pyridinio)aminomethylene]diphosphonate dianion and [(5‐methyl‐2‐pyridyl)aminomethylene]diphosphonate trianion in salts with 4‐aminopyridine and ammonia

The crystal structures of two salts, products of the reactions between [(5‐methyl‐2‐pyridyl)aminomethylene]bis(phosphonic acid) and 4‐aminopyridine or ammonia, namely bis(4‐aminopyridinium) hydrogen [(5‐methyl‐2‐pyridinio)aminomethylene]diphosphonate 2.4‐hydrate, 2C₅H₇N₂⁺·C₇H₁₀N₂O₆P₂²⁻·2.4H₂O, (I), and triammonium hydrogen [(5‐methyl‐2‐pyridyl)aminomethylene]diphosphonate monohydrate, 3NH₄⁺·C₇H₉N₂O₆P₂³⁻·H₂O, (II), have been determined. In (I), the Z configuration of the ring N—C and amino N—H bonds of the bisphosphonate dianion with respect to the C_ring—N_amino bond is consistent with that of the parent zwitterion. Removing the H atom from the pyridyl N atom results in the opposite E configuration of the bisphosphonate trianion in (II). Compound (I) exhibits a three‐dimensional hydrogen‐bonded network, in which 4‐aminopyridinium cations and water molecules are joined to ribbons composed of anionic dimers linked by O—H...O and N—H...O hydrogen bonds. The supramolecular motif resulting from a combination of these three interactions is a common phenomenon in crystals of all of the Z‐isomeric zwitterions of 4‐ and 5‐substituted (2‐pyridylaminomethylene)bis(phosphonic acid)s studied to date. In (II), ammonium cations and water molecules are linked to chains of trianions, resulting in the formation of double layers.     

Deformation of gradient shape as a result of preferential adsorption of solvents in mixed mobile phases

Gradient elution has been studied in typical normal and reversed-phase systems. Deformations of gradient profiles have been evidenced as a result of preferential adsorption of modifiers of the mobile phase. This phenomenon was pronounced in the normal-phase system, for which gradient profiles deviated significantly from those programmed. This influenced the retention and shapes of band profiles of the eluting solute. Hence, in order to predict gradient propagation correctly the adsorption equilibrium of modifiers has been quantified. Moreover, at low modifier content, deformations of band profiles of the solute has been registered as a result of the competitive adsorption in the system solute-modifier. This effect has been predicted by a competitive adsorption model. For the reversed-phase systems the influence of the modifier adsorption on gradient propagation was insignificant for typical mobile phases investigated. Therefore, the work has been focused on gradient predictions in the normal-phase system.     

Effect of heat treatment on the structure and morphology of ZnO nanorod array and its composite with titania precursor

ABSTRACT

Effects of the elevated temperature on the structure evolution of the ZnO nanorod array (ZNA) and their hybrid nanocomposite with layered (tetramethyl)ammonium titanate (LTMAT) prepared by the liquid phase deposition were investigated. The vertically oriented ZnO nanorods were deposited on a quartz plate by a chemical bath deposition method and then they were penetrated by the LTMAT using the dip-coating method from the water solution. As a result of such an experimental procedure, an assembly composed of the ZNA with LTMAT was obtained and called hybrid nanocomposite. Since the LTMAT converts to TiO₂ upon subsequent sintering at 350 °C, it can be regarded as TiO₂ precursor for the thermal treatment experiments. The experiments with ZNA and their hybrid nanocomposite at the elevated temperature revealed coalescence of the deposited ZnO nanorods and crystallization of zinc titanate with Zn₂TiO₄ stoichiometry.     

Surface Studies on Glass Powders Used in Commercial Glass-Ionomer Dental Cements

The surface properties of three commercial ionomer glass powders, i.e., Fuji IX, Kavitan Plus and Chemadent G-J-W were studied. Samples were analyzed by X-ray fluorescence spectroscopy (XRF), and the density was determined by gas pycnometry. Morphology was studied using scanning electron microscopy (SEM) and laser diffraction (LD) technique, whereas low-temperature nitrogen sorption measurements determined textural parameters like specific surface area and pore volume. Thermal transformations in the materials studied were evaluated by thermogravimetric analysis (TGA), which was carried out in an inert atmosphere between 30 °C and 900 °C. XRF showed that Fuji IX and Kavitan Plus powders were strontium-based, whereas Chemadent G-J-W powder was calcium-based. Powders all had a wide range of particle sizes under SEM and LD measurements. Specific surface areas and pore volumes were in the range 1.42–2.73 m²/g and 0.0029 to 0.0083 cm³/g, respectively, whereas densities were in the range 2.6428–2.8362 g/cm³. Thermogravimetric analysis showed that the glass powders lost mass in a series of steps, with Fuji IX powder showing the highest number, some of which are attributed to the dehydration and decomposition of the polyacrylic acid present in this powder. Mass losses were more straightforward for the other two glasses. All three powders showed distinct losses at around 780 °C and 835 °C, suggesting that similar dehydration steps occur in all these glasses. Other steps, which differed between glass powders, are attributed to variations in states of water-binding on their surfaces.     

Multiband processing of multimode light: combining 3D photonic lanterns with waveguide Bragg gratings

The first demonstration of narrowband spectral filtering of multimode light on a 3D integrated photonic chip using photonic lanterns and waveguide Bragg gratings is reported. The photonic lanterns with multi‐notch waveguide Bragg gratings were fabricated using the femtosecond direct‐write technique in boro‐aluminosilicate glass (Corning, Eagle 2000). Transmission dips of up to 5 dB were measured in both photonic lanterns and reference single‐mode waveguides with 10.4‐mm‐long gratings. The result demonstrates efficient and symmetrical performance of each of the gratings in the photonic lantern. Such devices will be beneficial to space‐division multiplexed communication systems as well as for units for astronomical instrumentation for suppression of the atmospheric telluric emission from OH lines.     

Gold Nanoparticles as Effective ion Traps in Poly(dimethylsiloxane) Cross-Linked by Metal-Ligand Coordination

At this time, the development of advanced elastic dielectric materials for use in organic devices, particularly in organic field-effect transistors, is of considerable interest to the scientific community. In the present work, flexible poly(dimethylsiloxane) (PDMS) specimens cross-linked by means of ZnCl₂-bipyridine coordination with an addition of 0.001 wt. %, 0.0025 wt. %, 0.005 wt. %, 0.04 wt. %, 0.2 wt. %, and 0.4 wt. % of gold nanoparticles (AuNPs) were prepared in order to understand the effect of AuNPs on the electrical properties of the composite materials formed. The broadband dielectric spectroscopy measurements revealed one order of magnitude decrease in loss tangent, compared to the coordinated system, upon an introduction of 0.001 wt. % of AuNPs into the polymeric matrix. An introduction of AuNPs causes damping of conductivity within the low-temperature range investigated. These effects can be explained as a result of trapping the Cl⁻ counter ions by the nanoparticles. The study has shown that even a very low concentration of AuNPs (0.001 wt. %) still brings about effective trapping of Cl⁻ counter anions, therefore improving the dielectric properties of the investigated systems. The modification proposed reveals new perspectives for using AuNPs in polymers cross-linked by metal-ligand coordination systems.     

Soluble Extracellular Polymeric Substances Produced by Parachlorella kessleri and Chlorella vulgaris: Biochemical Characterization and Assessment of Their Cadmium and Lead Sorption Abilities

In the present study, the potential of lead and cadmium removal by the extracellular polymeric substances (EPS) produced from Parachlorella kessleri and Chlorella vulgaris were investigated. Carbohydrates were the dominant components of EPS from both analyzed species. The contents of reducing sugars, uronic acids, and amino acids were higher in EPS synthesized by C. vulgaris than in EPS from P. kessleri. The analysis of the monosaccharide composition showed the presence of rhamnose, mannose and galactose in the EPS obtained from both species. The ICP-OES (inductively coupled plasma optical emission spectrometry) analyses demonstrated that C. vulgaris EPS showed higher sorption capacity in comparison to P. kessleri EPS. The sorption capacity of C. vulgaris EPS increased with the increase in the amount of metal ions. P. kessleri EPS had a maximum sorption capacity in the presence of 100 mg/L of metal ions. The FTIR analysis demonstrated that the carboxyl, hydroxyl, and carbonyl groups of EPS play a key role in the interactions with metal ions. The present study showed C. vulgaris EPS can be used as a biosorbent in bioremediation processes due to its biochemical composition, the presence of significant amounts of negatively charged uronic acids, and higher sorption capacity.     

Chemical Composition and Biological Activity of Argentinian Propolis of Four Species of Stingless Bees

The chemical composition of propolis of four species of stingless bees (SLBs) from Argentina was determined, and its antibacterial and anticancer activity was evaluated on selected types of microbes and cancer cell lines. Volatile secretions of all propolis samples are formed by 174 C₂–C₁₅ organic compounds, mainly mono- and sesquiterpenes and their derivatives. The chromatograms of ether extracts showed 287 peaks, of which 210 were identified. The most representative groups in the extracts of various propolis samples were diterpenoids (mainly resin acids), triterpenoids and phenolic compounds: long-chain alkenyl phenols, resorcinols and salicylates. The composition of both volatile and extractive compounds turned out to be species-specific; however, in both cases, the pairwise similarity of the propolis of Scaptotrigona postica and Tetragonisca fiebrigi versus that of Tetragona clavipes and Melipona quadrifasciata quadrifasciata was observed, which indicated the similarity of the preferences of the respective species when choosing plant sources of resin. The composition of the studied extracts completely lacked flavonoids and phenolcarboxylic acids, which are usually associated with the biological activity and medicinal properties of propolis. However, tests on selected microbial species and cancer cell lines showed such activity. All propolis samples tested against Paenibacillus larvae, two species of Bacillus and E. coli showed biofilm inhibition unrelated to the inhibition of bacterial growth, leading to a decrease in their pathogenicity. Testing the anticancer activity of ether extracts using five types of cell cultures showed that all four types of propolis studied inhibit the growth of cancer cells in a dose- and time-dependent manner. Propolis harvested by T. clavipes demonstrated the highest cytotoxicity on all tested cell lines.     

Influence of hybrid system of nanofillers on the functional properties of postconsumer PET‐G–based nanocomposites

In this article, postconsumer poly (ethylene glycol‐co‐1,4‐cyclohexanedimethanol terephthalate) (PET‐G) foils have been modified with three types of carbon nanofillers that differ in size and shape, ie, multiwalled carbon nanotubes (MWCNTs), graphene nanoplatelets (GNP), and nanosized carbon black (nCB), thus enabling the reusage of recyclate in receiving new functional materials. The series of polymer hybrid nanocomposites have been prepared via a two‐stage polycondensation process, be means of glycolysis of postconsumer PET‐G foil, followed by polycondensation in the presence of carbon nanofillers. The scanning electron microscopy revealed that nanoadditives were uniformly dispersed into the whole volume of polymer matrix. The results present the synergistic effect of hybrid system of nanofillers in improving tensile properties of PET‐G. It has been found that the incorporation of three types of carbon nanofillers has not affected the glass transition temperature of the polymer matrix. Moreover, the incorporation of carbon nanofillers, and the mixture of two, or even three of those, caused an improvement in thermal conductivity and thermal stability.     

Oligocarbazoles as ligands for lead-selective liquid membrane electrodes.

Oligocarbazoles have been applied as new ionophores in liquid membrane electrodes (ISEs) destined for lead(II) determination in water samples. The oligocarbazole-containing ISEs demonstrated a close-to-Nernstian potentiometric response towards Pb2+ in the activity range 10(-7)-10(-2) M. The selectivity coefficients measured by the matched potential method (MPM) confirmed their good selectivity against common interfering mono- and doubly charged cations. The oligocarbazole-containing ISEs do not respond towards protons. Their applicability has been checked by performing the recovery test while using a sample of wastewater.