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Volume 72, Nº 1 (2017)

Article

Crystal structure of 9-(5,5-dimethyl-2,4,5,6-tetrahydro-1H-phenalen-2-yl)-5,5,9-trimethyl-5,6,8,9-tetrahydrocyclopenta[a]phenalen-10(4H)-one

Banaru A., Smol’yakov A.

Resumo

The structure of 9-(5,5-dimethyl-2,4,5,6-tetrahydro-1H-phenalen-2-yl)-5,5,9-trimethyl-5,6,8,9-tetrahydrocyclopenta[а]phenalen-10(4H)-one was determined by X-ray crystallography. The intermolecular interaction energies were calculated by the atom-atomic approach for the crystal structure. The character of the crystal structure and the structural subclass were established.

Moscow University Chemistry Bulletin. 2017;72(1):1-5
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Cryochemical synthesis and antibacterial activity of a hybrid composition based on Ag nanoparticles and dioxidine

Vernaya O., Shabatin V., Semenov A., Shabatina T.

Resumo

Hybrid nanocomposites based on an dioxidine antimicrobial substance modified with silver were produced by means of cryochemical synthesis. TEM, UV-absorption spectroscopy, X-ray diffraction, and surface analysis based on low-temperature argon adsorption showed the formation of hybrid nanosystems consisting of drug substance particles with a size of 50–300 nm including internal small Ag nanoparticles with a size of 2–40 nm. The obtained hybrid nanosystems showed higher antibacterial activity against E. coli 52, S. aureus 144, and M. cyaneum 98 than did the original dioxidine.

Moscow University Chemistry Bulletin. 2017;72(1):6-9
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Total reflection X-ray fluorescence determination of rare earth elements in mineral water

Oskolok K., Monogarova O., Alov N.

Resumo

A method is proposed for determination of lanthanum, cerium, praseodymium, neodymium, and samarium in mineral water by means of total-reflection X-ray fluorescence analysis. In this work, the combined technique of preconcentration of rare earth ions is used. This technique consists of coprecipitation of metal hydroxides on the collector (iron (III) hydroxide) and dispersive liquid–liquid microextraction of their complexes with 1-(2-pyridylazo)-2-naphthol by chloroform in the presence of ethanol. The use of the developed hybrid approach allows simultaneous determination of the mentioned metals in mineral water in the range n(10–2–101) μg/L. The results of analysis of Arkhyz and Rychal-Su mineral waters by the proposed extraction–X-ray fluorescent method are confirmed by the literature data, obtained by inductively coupled plasma mass spectrometry.

Moscow University Chemistry Bulletin. 2017;72(1):10-14
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Crucible atomizer for determining dissolved and suspended forms of elements in natural waters

Oreshkin V., Tsysin G.

Resumo

A model of a specialized microcolumn has been proposed and tested, namely, a crucible atomization microcolumn for electrothermal atomic absorption analysis of natural waters in which the zone of isolation of suspended matter and the zone of dynamic preconcentration of dissolved forms of elements are separated. A direct independent analysis of solid suspended matter and DETATA concentrate is possible upon completion of preconcentration. Such an approach is used to determine suspended and dissolved forms of cadmium and lead in river water and soil groundwater.

Moscow University Chemistry Bulletin. 2017;72(1):15-18
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Reflectance spectra of organic matrices on the basis of photonic crystals formed of polystyrene microspheres with a particle size of 230 nm

Ivanov A., Kozlov A., Koreshkova A., Abdullaev S., Fedorova I.

Resumo

The specular and diffuse reflectance spectra of organic matrices on the basis of photonic crystals formed of polystyrene microspheres with a particle size of 230 nm and polydimethylsiloxane layers, which are both applied on substrates made of quartz glass and acrylic plates, are recorded. Part of the organic matrix changes color from green to red-yellow 2 to 5 min after contact with a nonpolar solvent. The kinetics of structural changes occurring in the organic matrix under the influence of non-polar organic solvents, such as toluene, benzene, and n-hexane, is studied by diffusion reflectance spectroscopy. The equilibria in the organic matrix are achieved in 15–20 min.

Moscow University Chemistry Bulletin. 2017;72(1):19-23
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4-amino-2-phenylindole-based compounds with potential antibacterial activity

Alyamkina E., Stepanenko I., Yamashkin S., Yurovskaya M.

Resumo

Primary condensation of 4-amino-2-phenylindole with ethyl acetoacetate and 4,4,4-trifluoroacetoacetate resulted in corresponding amides, which under acidic conditions were converted to pyrrolo[2,3-h]quinolones. Antibacterial activity of the amide obtained from aminoindole and ethyl 4,4,4-trifluoroacetylacetate was detected.

Moscow University Chemistry Bulletin. 2017;72(1):24-28
pages 24-28 views

Sonocatalytic oxidative desulfurization of oil from the Zhanazhol oilfield

Kairbekov Z., Anisimov A., Myltykbaeva Z., Kanseitova D., Rakhmanov E., Seisembekova A.

Resumo

Sonocatalytic oxidative desulfurization of oil from the Zhanazhol oilfield was investigated. Application of stepwise periodic treatment in an ultrasound field in the presence of a Ni-skeletal catalyst and oxidizer was shown to be an effective procedure for improving the quality of oil and oil-based products, which allowed targeted change of its chemical composition, increasing the yield of light products (gasoline and diesel fractions from 15.6 to 21.9 and from 47.7 to 58.6 wt %, respectively) and decreasing the sulfur content in oil products to 49%.

Moscow University Chemistry Bulletin. 2017;72(1):29-33
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Studies of aminolysis of acrylonitrile–divinylbenzene–methyl methacrylate copolymers

Balanovsky N., Cherednichenko A.

Resumo

Aminolysis of nitrilacrylate–divinylbenzene–methyl methacrylate copolymers by diethylenetriamine is studied under various conditions. The effect of temperature and catalyst concentration on the properties of synthesized anion exchangers depending on the duration of aminolysis is investigated. The conditions for synthesizing anion exchangers with high capacity characteristics are proposed according to the study results.

Moscow University Chemistry Bulletin. 2017;72(1):34-37
pages 34-37 views

Stabilized phospholipid dispersions based on organosilicon amphiphiles

Sarychev G., Mironova M., Budanova U., Sebyakin Y.

Resumo

Cerasome-forming amphiphile based on L-aspartic acid dihexadecyl ester derivative with (3-aminopropyl) triethoxysilane moiety in its structure was synthesized. Mixed storage-stable lipid dispersions containing phosphatidylcholine were prepared and their properties were examined.

Moscow University Chemistry Bulletin. 2017;72(1):38-41
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Ultrasound-assisted synthesis of nanostructured transition metal oxides

Romanovsky B., Maerle A., Karakulina A., Moskovskaya I.

Resumo

Ultrasound pretreatment of aqueous solutions of cetyltrimethylammonium bromide as a structure- directing agent has been applied to prepare nanostructured mesoporous Mn, Fe, and Ni oxides. After removal of the template by triple extraction with a water–ethanol solution of sodium acetate or ammonium chloride, air-calcined samples of oxide materials prepared in such a way possess surface areas of about 300–450 m2/g and are thermally stable up to 300°C.

Moscow University Chemistry Bulletin. 2017;72(1):42-48
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The use of the ratios of intensities of spectral lines for X-ray fluorescence analysis of metal alloys and oxide materials

Garmay A., Oskolok K., Monogarova O.

Resumo

An X-ray fluorescence analysis technique is proposed, which is based on using ratios of intensities of spectral lines. The technique includes performing calculations for evaluation of calibration equations, which allows using few reference samples or carrying out standardless analysis, if necessary. That parameters of the calibration equations depend linearly on concentrations of disturbing elements allows one to simplify taking their influence into account. To apply the developed technique to analysis of samples containing a significant amount of undetectable light elements, a use of a dependence of intensity ratio of the characteristic radiation of the X-ray tube’s anode, coherently and incoherently scattered by a sample, on a total content of undetectable elements is proposed. The technique’s adequacy is demonstrated by analysis of standard steel samples, metal cuttings and iron-ore materials.

Moscow University Chemistry Bulletin. 2017;72(1):49-55
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Determination of the enantiomeric purity of albuterol on sorbents modified by macrocyclic antibiotics

Shapovalova E., Fedorova I., Priporova A., Ananieva I., Shpigun O.

Resumo

The separation of albuterol enantiomers on sorbents with macrocyclic glycopeptide antibiotics immobilized on the silica surface was investigated. Commercial columns—Nautilus-E (BioKhimMak, Russia) with eremomycin as a chiral selector and ChirobioticTAG (Astec, United States) with teicoplanin aglycone as a chiral selector—were used for enantioseparation. Levalbuterol is the (R)-enantiomer of albuterol. We managed to separate albuterol enantiomers on both columns in a polar organic mode, but selectivity was higher on the ChirobioticTAG column (Rs = 1.7). The maximum resolution of enantiomer peaks (1.7) was observed in methanol–acetonitrile–triethylamine–acetic acid (90: 10: 0.05: 0.05) as the mobile phase. The detection limit of the compound calculated by a signal–background ratio of 3: 1 was 0.00002 mg/mL, which corresponds to 0.1% of (S)-enantiomer with respect to the total amount. The results made it possible to determine the enantiomeric purity of the active pharmaceutical substances of levalbuterol.

Moscow University Chemistry Bulletin. 2017;72(1):56-62
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Rapid assessment of soil pollution with kerosene using a carbon-nanotube-based piezosensor

Kotchetova Z., Kuchmenko T., Bazarsky O.

Resumo

The possibility of determining the kerosene content in the ground using a flash detector with open cell detection based on a piezosensor is considered. The coating of the electrodes of a quartz crystal resonator and its weight for the detection of kerosene vapors in a wide concentration range, the structural parameters of the flash detector housing, the conditions for detecting kerosene vapors above ground are optimized. The accuracy and reliability of assessing of the level of kerosene contamination in different types of soils are estimated in field conditions.

Moscow University Chemistry Bulletin. 2017;72(1):63-68
pages 63-68 views