Thermal and spectral analysis of copolymers with sulphur groups

Journal of Thermal Analysis and Calorimetry - The paper presents the synthesis, structure and polymerization of S-phenyl 2-methylprop-2-enethioate (PSM). This compound was prepared in the reaction...     

Regioselective formation of β‐(E)‐ and α‐alkenylsilane moiety attached to silsesquioxane core via Pt‐ and Ru‐based hydrosilylation

The first attempts to use ethynylsiloxysilsesquioxanes as reagents for hydrosilylation in the presence of Pt‐ and Ru‐based catalysts are reported. The results obtained strongly depend on the catalytic system used. The catalysts are proved to promote regioselective introduction of β‐(E)‐ and α‐fragments of the alkenylsilane group to the silsesquioxane core. The favourable features of these catalytic systems are their high selectivity and the requirement for relatively mild conditions. This methodology was also successfully applied to dihydro‐substituted organosilicon compounds to obtain a new class of silsesquioxane‐based compounds.     

Amino-Modified Silicate Xerogels Complexed with Cu(II) as Catalyst Precursors. Coordination State and Thermal Decomposition

The sol-gel process is a useful method for preparing two series of organically and co-ordinately modified xerogels of the types [CuN _n ]·N _5–n ·5xSiO_4/2 (n < 4) and [Cu(N–N)_n]·(N–N)_2–n ·2x SiO_4/2(n 2), where N = NH₂(CH₂)₃ SiO_3/2, N–N = NH₂(CH₂)₂NH·(CH₂)₃SiO_3/2 and x = [SiO_4/2]/[N] or [SiO_4/2]/[N–N]. The amino groups in the materials are coordinately active and participate partly in the coordination sphere of Cu(II) ions. The composition of the coordination sphere can be varied with the SiO_4/2 content and also as a result of the thermal decomposition of the organic residues at higher temperatures.Because the xerogel materials are considered to be catalyst precursors, this study is focused on their coordination and thermal properties. The prepared xerogels, such as silica, aminated silicates with N and N–N, as well as those entities complexed with Cu(II), were characterised by FT-IR spectroscopy. During gelation and thermal decomposition the materials were analysed by electron paramagnetic resonance (EPR) spectroscopy. The xerogels were additionally studied by UV-Vis absorption spectroscopy. The gaseous products of the thermal decomposition of these materials in an Ar atmosphere were investigated by the use of FT-IR spectroscopy coupled with TG and DTG thermal analysis. These data were complemented by temperature-programmed decomposition (TPDec) in a 2% O₂ + 98% Ar stream coupled with quadrupole mass spectroscopy.     

Monodisperse magnetic poly(glycidyl methacrylate) microspheres for isolation of autoantibodies with affinity for the 46 kDa form of unconventional Myo1C present in autoimmune patients

Monodisperse nonmagnetic macroporous poly(glycidyl methacrylate) (PGMA) microspheres were synthesized by multistep swelling polymerization of glycidyl methacrylate, ethylene dimethacrylate and 2-[(methoxycarbonyl)methoxy]ethyl methacrylate (MCMEMA). This was followed (a) by ammonolysis to modify the microspheres with amino groups, and (b) by incorporation of iron oxide (γ-Fe₂O₃) into the pores to render the particles magnetic. The resulting porous and magnetic microspheres were characterized by scanning and transmission electron microscopy (SEM and TEM), atomic absorption and Fourier transform infrared spectroscopy (AAS and FTIR), elemental analysis, vibrating magnetometry, mercury porosimetry and Brunauer-Emmett-Teller adsorption/desorption isotherms. The microspheres are meso- and macroporous, typically 5 μm in diameter, contain 0.9 mM · g^?1 of amino groups and 14 wt.% of iron according to elemental analysis and AAS, respectively. The particles were conjugated to p46/Myo1C protein, a potential biomarker of autoimmune diseases, to isolate specific autoantibodies in the blood of patients suffering from multiple sclerosis (MS). The p46/Myo1C loaded microspheres are shown to enable the preconcentration of minute quantities of specific immunoglobulins prior to their quantification via SDS-PAGE. The immunoglobulin M (IgM) with affinity to Myo1C was detected in MS patients.

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Graphical abstract Monodisperse magnetic poly(glycidyl methacrylate) microspheres were synthesized, conjugated with 46 kDa form of unconventional Myo1C protein (p46/Myo1C) via carbodiimide (DIC) chemistry, and specific autoantibodies isolated from blood of multiple sclerosis (MS) patients; immunoglobulin M (IgM) level increased in MS patients.

     

Effect of Re addition on the crystallization,heat treatment and structure of the Cu–Ni–Si-Cr alloy

Differential scanning calorimetry (DSC) was used to investigate the thermal behavior and non-isothermal crystallization kinetics of the Fe₆₇Nb₅B₂₈ metallic glasses prepared by melt-spinning method. DSC traces exhibit that the crystallization takes place through a single exothermic reaction, and it processes a good thermal stability in thermodynamics. The activation energies for nucleation and grain growth processes were calculated to be 536 ± 22 and 559 ± 20 kJ mol^?1 by Kissinger equation, respectively, and 551 ± 24 and 574 ± 20 kJ mol^?1 by Ozawa equation, respectively. It means that the grain growth process is more difficult than the nucleation process. The variation of local Avrami exponent n(x) with crystallized fraction x demonstrates that the crystallization mechanism varies at different stages. The n(x) is larger than 2.5 at the initial stage of 0 < x < 0.3, implying a mechanism of diffusion-controlled three-dimensional growth with increasing nucleation rate. The n(x) decreases from 2.5 to 1.5 in the range of 0.3 < x < 0.65, suggesting that the crystallization belongs to three-dimensional nucleation and grain growth with decreasing nucleation rate. And n(x) lies between 1.0 and 1.5 in the range of 0.65 < x < 0.95, indicating that the crystallization corresponds to the growth of particles with an appreciable initial volume. Low-temperature annealing corresponds to the precipitation of α-Fe, Fe₂B, and Fe₂₃B₆ phases, and further annealing leads to the formation of α-Fe, Fe₂B, and FeNbB phases. The magnetic properties in relation to microstructure change of the Fe₆₇Nb₅B₂₈ metallic glasses are discussed.     

Facilitated transport of palladium(II) across polymer inclusion membrane with ammonium ionic liquid as effective carrier

This work focuses on the application of polymer inclusion membrane (PIM) with tricaprylmethylammonium thiosalicylate, [A336][TS] (TOMATS), a thiol-containing task-specific ionic liquid for the transport of Pd(II) ions from aqueous solutions. 0.3 M thiourea in 0.1 M hydrochloric acid was found the most effective stripping phase in the transport of Pd(II) from membrane phase containing TOMATS. Separation of Pd(II) ions was also carried out from hydrochloric acid solution containing Pt(IV), Fe(III), Ni(II), and Mn(II). Pd(II) ions were preferably transported in the presence of these metal ions. The separation coefficients followed the order: S _Pd/Pt < S _Pd/Fe < S _Pd/Ni < S _Pd/Mn. [A336][TS] proved to be an excellent ion carrier for Pd(II) from hydrochloric acid solution. The results also showed that transport efficiency of the PIM was reproducible and it can be useful for the development of the simple and highly effective method of Pd(II) recovery from leach liquor of spent catalysts.     

Synthesis of β-cyclodextrin-lysozyme conjugates and their physicochemical and biochemical properties

Recently a great interest in the field of protein engineering and the design of innovative drug delivery systems employing specific ligands such as cyclodextrins is observed. The paper reports the solid state, thermal method for protein coupling with β-cyclodextrin and the physicochemical and biological properties of the obtained conjugates. The structure of the obtained conjugates was investigated via liquid chromatography-mass spectrometry, dynamic light scattering and circular dichroism analysis. The presented conjugates were biologically active and covalently bound β-cyclodextrin preserved the ability to form inclusion complexes with the model compound. This report demonstrates the great potential of cyclodextrin as a modifying unit that can be used to modulate the properties of therapeutic proteins, additionally giving such conjugates the possibility to transport many therapeutic substances in the form of inclusion complexes. In addition, the paper presents the potential of protein-cyclodextrin conjugates to construct innovative bioactive molecules for biological and medical applications.     

Chromatographic and spectroscopic investigation of the associative changes with the selected higher fatty alcohols

An attempt was made to compare usefulness of the ir spectroscopic technique with paper chromatography in the investigations concerning self-association of higher fatty alcohols. A conclusion was drawn that only the complementary application of both analytical methods better enabled to trace the establishing of association equilibria in the given experimental conditions.     

Functions related to convexity and smoothness of normed spaces

We introduce a few functions related to convexity and smoothness of normed spaces. Those functions turn out to be moduli of convexity or smoothness or play an intermediate role. We calculate the exact formulas for introduced functions in some classical Banach spaces. An application to geometry of normed spaces is also indicated.     

Quasi-arithmetic-type invariant means on probability space

Aequationes mathematicae - For a family $$(\mathscr {A}_x)_{x \in (0,1)}$$ of integral quasi-arithmetic means satisfying certain measurability-type assumptions we search for an integral mean K such...