Three-component catalytic method for synthesis of α-amino phosphonates with the use of α-amino acids as amine component

Interaction of aliphatic and aromatic aldehydes and ketones with optically active L-α-amino acids or their esters in the three-component catalytic one-pot synthesis of α-aminophosphonates was studied. The corresponding α-amino phosphonates are formed in high yields as mixtures of diastereomers. Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 4, pp. 768–774, April, 2007.     

Resonance Rayleigh scattering determination of trace amounts of Al in natural waters and biological samples based on the formation of an Al(III)-morin-surfactant complex

A novel method for the determination of trace amounts of Al(III) based on resonance Rayleigh scattering (RRS) has been developed. In the presence of some surfactants, Al(III) can react with morin and form an Al(III)-morin-surfactant complex, which results in the enhancement of RRS intensity and the appearance of the corresponding RRS spectral characteristics. Their maximum scatter peaks are at 476 nm for the cetyltrimethylammonium bromide (CTAB) system, 489 nm for the cetylpyridinium chloride (CPC) system, 474 nm for the Triton X-100 system, and 473 nm for the Tween-20 system. The enhanced RRS intensity is directly proportional to the concentration of Al(III). The detection limits are in the range of (0.50-1.2)×10⁻⁷ mol l⁻¹ depending on the surfactant. The characteristics of RRS spectra of the complexes, the optimum conditions of these reactions and the influencing factors have been investigated. The method has high selectivity, and was successfully applied to the determination of Al(III) in natural and biological samples. Furthermore, according to different complexation capacity of Al(III)-morin-CTAB system under two pH conditions, speciation analysis of Al(III) in natural waters was explored. The labile monomeric Al fraction (mainly inorganic Al, Al_i) is determined at acidic pH and the total monomeric Al fraction (Al_a) is determined at alkaline pH. The results are in agreement with those obtained by Driscoll’s 8-hydroxyquinoline extraction-ion exchange method.     

Triterpenoids from plants of the genus Tamarix

The taraxeran-14-ene-type triterpenoids methyl 3-β-al-D-fridoolean-14-en-28-oate (1), 3-α-[3″,4′-dihydroxytrans-cinnamoyl]-oxy-D-fridoolean-14-en-28-oic acid (2), and β-sitosterol (3) were isolated from the aerial part of plants from the genus Tamarix (T. laxa, T. elongata) (Tamaricaceae). The structures of the triterpenoids were proved using spectral data (IR, UV, PMR, ¹³C NMR, 2D NMR ¹H-¹H COSY, HMQC, HMBC, mass). Compound 1 is new and not previously described in the literature. __________ Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 271–273, May–June, 2006.     

东太平洋深海锰结核的化学元素研究

用ICP-AES法测定了东太平洋深海锰结核样品中二十多种主，次及微量元素，结果表明，表面瘤状和表面光滑两种类型锰结核的化学元素含量有较明显的区别，如表面光滑的锰结核TiO2含较高，而表面瘤状的锰结核Mn/Fe之值较高等。     

Determination of hydroxycarbamates in aqueous matrices by direct derivatization and GC-MS analysis in chemical ionization mode

A rapid and effective procedure, developed for the determination of polar compounds in water, has been applied to hydroxycarbamates. In few minutes, it is possible to perform a catalyzed derivatization of such compounds directly in the aqueous medium, using n-hexyl chloroformate. Extraction with n-hexane and injection into a benchtop GC-MS system are the only two further steps to complete the analysis. Chemical ionization proved to be more effective than electron impact to produce valuable mass spectra in terms of selectivity and sensitivity. Linear quantitative responses were demonstrated over a two-order-of-magnitude range. The minimum detectable concentration was 3 ppb for acetohydroxamic acid and 10 ppb for hydroxyurethane, obtained from Po river water samples spiked with the two hydroxycarbamate standards.     

微量热法研究γ-Mo2N催化剂表面氢的微分吸附热

Differential heats of H 2 adsorption on γ-Mo2N catalysts were studied by using microcalorimetry. Samples with high and medium surface areas (90 and 17 m2•g -1 ) present a homogeneous energetic distribution of surface sites, which corresponds with the preferential orientation of their (200) planes. Molybdenum nitride with low surface area (8 m2•g -1 ) displays a heterogeneous energetic distribution of H 2 adsorption sites. The higher initial differential heat of hydrogen adsorption observed for the low surface Mo nitride was attributed to species adsorbed on surface sites associated with the (111) plane.     

Chemical separation and inductively coupled plasma–atomic emission spectrometric determination of seventeen trace metals in thorium oxide matrix using a novel extractant – Cyanex-923

Comprehensive studies have been carried out on the extraction behaviour of thorium matrix vis-a-vis 17 trace metallic elements using a novel extractant viz. Cyanex-923. The near total extraction of thorium and quantitative separation of these metals has been established using inductively coupled argon plasma–atomic emission spectrometry (ICP–AES). The recovery of few representative elements has been confirmed by radio-active tracer studies. The studies carried out here have enabled determination of μg/l amounts of all analyte elements with a precision of better than 1% RSD with prior chemical separation from as low as 1 g thorium sample in just five chemical extractions.     

硫化物/Ru(II)络合物复合敏化TiO2纳米多孔膜

用光电化学方法研究了ＣｄＳ,ＰｄＳ和Ｒ１１Ｌ２（ＮＣＳ）２,（Ｌ＝２,２′－ｂｉｐｙｄｉｎｅ－４,４′－ｄｉｃａｒｂｏｘｙｌｉｃａｃｉｄ）复合敏化ＴｉＯ２纳米晶电极的光电化学行为,结果表明,采用复合敏化比用Ｒ１１（ＩＩ）络合物单独敏化ＴｉＯ２纳米晶电极效果好,大大提高了光电转换效率,主要原因是采用复合敏化,可防止ＴｉＯ２导带上由光注入产生的电子的反向转移,避免了电子的损失。     

Effect of the complex forming ion on the physicochemical characteristics of solvation of tetraphenylporphine complexes

The enthalpies of dissolution, transfer, and axial coordination for the Cd(II), Co(II), Mn(III), Fe(III), and Cr(III) complexes of tetraphenylporphine, H₂(TPP), in nonpolar (C₆H₆, CCl₄) and electron-donating solvents (DMF, DMSO, Py,c-C₅H₁₀NH) have been determined calorimetrically at 298.15 K. On the basis of thermogravimetrical data for the corresponding crystallosolvates the composition, thermal stability, and energy of intermolecular interaction of the metal-porphine complexes with pyridine have been calculated. Complexing in noncoordinating solvents brings about no radical change in the physicochemical characteristics of axial coordination which depend critically on the electron structure of the complex-forming metal.Translated fromfzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 5, pp. 846–850, May, 1993.     

利用无水乙醇分解制备碳纳米管

利用CVD法高温分解无水乙醇,以分子筛（合成皂石）基体上的Fe颗粒为催化剂,制备出了管壁更薄、端部为开口结构的碳纳米管.本实验制备出的碳纳米管,相对于传统CVD方法制备出的碳纳米管,在实验条件控制稳定的情况下,管壁较直、缺陷较少、管内径较大.具有这样结构的碳纳米管在储氢等方面应具备更为优良的效果,从而有着潜在的应用前景.