Influence of surface modified TiO2 nanoparticles by gallates on the properties of PMMA/TiO2 nanocomposites

Nanocomposites based on poly(methyl methacrylate) (PMMA) and TiO₂ nanoparticles were synthesized by in situ radical polymerization of MMA in solution. The surface of TiO₂ nanoparticles was modified with four gallic acid esters (octyl, decyl, lauryl and cetyl gallate). The content of gallates present on the surface of TiO₂ was calculated from the TGA results. The influence of length of hydrophobic tail of amphiphilic alkyl gallates on dispersability of surface modified TiO₂ nanoparticles in PMMA matrix, the molecular weight and glass transition temperature of PMMA, as well as the thermal stability of the prepared PMMA/TiO₂ nanocomposites in nitrogen and air was investigated. The influence of content of TiO₂ nanoparticles on the properties of these nanocomposites was also examined. The formation of a charge transfer complex between the surface Ti atoms and the gallates was confirmed by FTIR and UV spectroscopy. TEM micrographs of the PMMA/TiO₂ nanocomposites revealed that degree of TiO₂ aggregation can be significantly lowered by increasing the length of aliphatic part of the used gallates. The molecular weight of PMMA slightly decreases with the increase of TiO₂ content, indicating that used TiO₂ nanoparticles act as radical scavengers during the polymerization of MMA. The presence of surface modified TiO₂ nanoparticles do not have an influence on the mobility of PMMA chain segments leading to the same values of glass transition temperature for all investigated samples. Thermal and thermo-oxidative stability of the PMMA matrix are improved by introducing TiO₂ nanoparticles modified with gallates.     

Electronic spectra of Cu(II) crystal complexes with S-methylthiosemicarbazones

Electronic spectra for a series of coordination compounds of copper(II) with tridentant ligands of salicyl aldehyde S-methylthiosemicarbazone and 8-quinoline aldehyde S-methylthiosemicarbazone were investigated. Coordinations of central ions were determined on the basis of X-ray data and IR spectra. Electronic transitions were detected by processing the diffusion-reflection spectra according to theKubelka-Munk theory. Identifications proved the presence of bands corresponding to intraligand transition, charge transfer spectra and the transition of d-d type which are the result of the elimination of d-orbital degeneration for Cu(II) ions in the crystal field. The effect of the symmetry of coordination polyhedrons is discussed.

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Elektronenspektren von Cu(II) Kristall-Komplexen mit S-Methylthiosemicarbazonen

Zusammenfassung Es wurden Elektronenspektren einer Serie von Koordinationsverbindungen des Kupfer(II) mit tridentaten Liganden (Salizylaldehyd-S-methylthiosemicarbazon und 8-Chinolinylaldehyd-S-methylthiosemicarbazon) untersucht. Die Zentralionkoordination wurde durch Röntgenstrahlenuntersuchungen und auf Grund der IR-Spektren festgestellt. Die Elektronenübergänge wurden nach derKubelka-Munk-Theorie aus den diffusen Reflexionsspektren ermittelt. Die Banden wurden den Intraligandübergängen, dem charge-transfer-Spektrum und den d-d-Typ-Übergängen, die als Resultat der Entartungsbeseitigung der Cu(II)-d-Orbitale im Kristallfeld verschiedener Symmetrie entstehen, zugeschrieben.

     

A simulation of neutron interaction from Am–Be source with the CR-39 detector

Presented in this paper is a simulation of the interaction of neutrons emitted from a cylindrical Am–Be source with a CR-39 detector. A Fortran90 program, called Neutron.f90, has been written to determine the specifications of secondary particles (alpha particle or proton) and the kinematics of the interactions. A Monte Carlo method was used to simulate which interactions occurred with the constituents of the CR-39 detector, H, C and O atoms. Due to the detector composition, elastic and nonelastic scattering of neutrons is possible. In this paper, nonelastic scattering includes: inelastic scattering; the emission of an alpha particle (n,α) reaction and the emission of a proton (n,p) reaction. Cross sections of other reactions are very small and negligible in comparison with the above mentioned. The energy deposited per unit mass per one neutron was calculated. In addition the contribution to the energy deposited by the alpha particles and protons were determined separately. The program Neutron.f90 computes the coordinates of points in which interactions occur i.e. where secondary particles appear. The energy and angular distributions of protons are also represented in this paper. Another Fortran90 program, called Track_Visibility.f90, was written to calculate the number of visible proton tracks and to calculate the energy deposited per one neutron per one visible track.     

1,5-Shift of hydrogen from carbon to carbon in the lead tetraacetate oxidation of 5,5-dimethyl-2-heptanol

By using α-deuteriated substrate, it was established that in the thermal lead tetraacetate reaction (in benzene) of 5,5-dimethyl-2-heptanol (1) oxidation to the corresponding ketone 4 proceeds not only by way of direct elimination of the carbinol (α) hydrogen, but also, to the extent of 43·-5%, by a route which involves 1,5-transfer of hydrogen from the carbinol (α) carbon atom to the ?-C atom.     

Simultaneous determination of N-unsubstituted and N-substituted nitroazoles and criteria for their identification-III Chromatographic separation and polarographic determination of halo-nitroimidazoles

Methods for identifying and determining halo-nitroimidazoles appearing together during synthetic processes, regardless of the preparation methods, are proposed. Polarographic determination can be used in all synthetic processes when halo-nitroimidazoles have been obtained by nitration of the halo-imidazoles. When the halo-nitroimidazoles have been obtained from 5(4)-halo-4(5)-nitroimidazoles by substitution of the imino hydrogen atom, and when only one N-substituted derivative has been obtained in a reaction mixture, simultaneous polarographic determination of both compounds is possible, but only when an alkaline medium is used as supporting electrolyte. In some cases, simultaneous polarographic determination of all three compounds present in a reaction mixture during N-substitution processes [one 5(4)-halo-4(5)-nitroimidazole and two N-substituted isomers] is also possible with alkaline supporting electrolyte. Explanations are given of the phenomena on which the simultaneous polarographic determination is based. When simultaneous polarographic determination cannot be used to determine the amount of each polarographically-active compound present in a reaction mixture, the compounds can be separated chromatographically and then determined individually by polarography.     

Synthesis and characterization of two Ni(II) complexes with furfural s-methylthiosemicarbazone

Synthesis of two Ni(II) complexes with furfural S-methylthiosemicarbazone (HL) of the formula [Ni(HL)₂(H₂O)₂](ClO₄)₂ (A) and [Ni(HL)₂(ClO₄)₂] (B) are reported. Compound A was obtained from an ethanolic solution of Ni(ClO₄)₂·6H₂O and HL, whilst compound B was produced by heating compound A to 378 K. An X-ray analysis of the complex A showed that it has a trans(H₂O)-trans(HL) octahedral configuration in which HL behaves as a bidentate (NN) ligand. On the basis of the IR and electronic spectra as well as the magnetism, it was found that the compound B has also an octahedral configuration in which, HL and ClO₄ groups, are coordinated.     

Ecological studies of the naturally occurring radionuclides, 137Cs and heavy metals in soil,plants and milk in surrounding of Kragujevac city,Serbia

Journal of Radioanalytical and Nuclear Chemistry - Vertical distribution of natural radionuclides, 137Cs and heavy metals were measured in soil and plants collected from Kragujevac surroundings....     

Coordination and Activation of the BF Molecule

No CO : Fluoroborylene (BF), isoelectronic with CO and N₂, can be trapped by a transition metal. The structurally characterized complex [{CpRu(CO)₂}₂(μ‐BF)] contains an unsupported bridging BF ligand, which is unprecedented in the structural chemistry of CO. With AlCl₃ , metal‐bound CO coordinates through the O atom without bond rupture, while the more polar and less π‐bonded BF ligand is heterolytically cleaved (see picture).

     

A preliminary survey of natural radionuclides in soil and indoor radon in the town of Niš, Serbia

Journal of Radioanalytical and Nuclear Chemistry - The activity concentration of natural radionuclides in the samples of soil from the town of Ni? were measured using the gamma spectroscopy...