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.     

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.     

On Kirk's asymptotic contractions

Recently Kirk introduced the notion of asymptotic contractions on a metric space and using ultrapower techniques he obtained an asymptotic version of the Boyd-Wong fixed point theorem. In this paper we extend this result and moreover, we give a constructive proof of it. Furthermore, we obtain a complete characterization of asymptotic contractions on a compact metric space. As a by-product we establish a separation theorem for upper semicontinuous functions satisfying some limit condition.     

Kerogen as a geochemical marker of the thermal history of rocks

The study presents examples of the application of oxyreactive thermal analysis to the geological prospecting of bitumen deposits. Thermal analysis performed under properly chosen analytical conditions allows determination of characteristic features of organic matter and, at the same time, estimation of the thermal history of rocks. Thermal oxyreactivity curves document whether rocks were heated before or not. The results of the oxyreactive thermal analysis correlate well with the results of routine chemical analyses of organic matter (e.g. the composition of kerogen and bituminous fraction, Rock-Eval analysis and others). Our study clearly demonstrates that the composition of organic matter in facially, lithostratigraphically, and biogenetically identical rocks depends on their thermal history.     

Alkylation of the inverted porphyrin nickel(II) complex by dihalogenalkanes: formation of monomeric and dimeric derivatives

An efficient and simple method of modification of "inverted" porphyrin is provided by reactions of 5,10,15,20-tetraaryl-2-aza-21-carbaporphyrinatonickel(II) 2 with dihalogenalkanes under basic conditions. The substituents are bound to the internal carbon or external nitrogen of the inverted pyrrole depending on dihalogenalkane and basic catalyst. The monomeric 2- or 21-ethoxymethyl-substituted species are formed in the reaction of 2 with dihalomethanes and sodium ethoxide or ethanol in the presence of K(2)CO(3). A novel, dimeric 21,21'-ethylene-linked derivative 11 is obtained from 2 and ethylene bromide in dichloromethane in the presence of potassium carbonate end ethanol, while application of potassium tert-butoxide promotes formation of N-bromoethyl-substituted monomer 12. Reaction of 2 with propylene bromide in the presence of proton scavenger efficiently leads to the 21-allyl-substituted monomer 14 that is a product of the HBr elimination from a transient 21-bromopropyl-substituted species. The new compounds have been identified and characterized by means of mass spectrometry and optical and NMR spectroscopies. A single-crystal X-ray analysis performed for 12 allows discussion of structural parameters concerning the macrocycle and coordination core. Formation of deprotonated species [2](-), which is proposed as a key intermediate in the alkylation reaction, has been observed spectroscopically. Chirality of the N-substituted derivatives induced by protonation of the internal carbon is observed by NMR at low temperatures.