Separation of isomers of saturated polycyclic hydrocarbons in packed capillary columns with graphitized thermal carbon black

Summary Using the example of perhydrophenanthrene, perhydroanthracene and cyclopentanodecalin isomers a possibility is shown to use packed capillary columns containing graphitized thermal carbon black for a complete separation of high-boiling mixtures of polycyclic saturated hydrocarbon isomers in accordance with the geometric structure of their molecules.     

高负载率纳米Pt-Ru/C催化剂的制备和表征

以Vulcan XC-72R碳黑为载体, 通过在含十二烷基硫酸钠(SDS)的乙二醇溶液中直接还原氯铂酸和三氯化钌, 制备了负载率为60%的纳米PtRu/C催化剂. 透射电镜(TEM)和X射线衍射(XRD)分析结果表明, SDS的加入可显著改善PtRu纳米颗粒在载体表面分散性, 平均粒径达到2.7 nm. 电化学循环伏安法(CV)测试的结果显示, 利用这种方法制备的纳米PtRu/C催化剂对于甲醇氧化具有较强的抗中毒能力和较高的电催化活性.     

Asymmetric Reductive Alkylation of Alanylproline by the Ethyl Esters of 4-Substituted 2-Oxobutenoic Acids

A method was developed for the synthesis of N-[1-(S)-(ethoxycarbonyl)-3-phenylpropyl]alanylproline (enalapril) by reductive alkylation of alanylproline with ethyl 2-oxo-4-phenylbutenoate under the conditions of hydrogenation in the presence of palladium black and 1.6% Pd/C. The yield of enalapril amounted to 65%. With the ethyl ester of the -oxo acid the diastereoselectivity of formation of the S,S,S-diastereomer was higher than with the saturated synthon. It is assumed that with ethyl 2-oxo-4-phenylbutenoate as synthon a conformationally restricted surface complex is formed between the unsaturated synthon and the active centers of the catalyst. During reductive alkylation of alanylproline by ethyl 2-oxo-4-(2-thienyl)butenoate poisoning of the catalyst occurs.     

活性炭纤维电极电解法处理墨绿B染料废水

将铁丝缠绕在活性炭纤维(简称ACF)上制成电极,并在阴极鼓入空气,用电解生成的Fenton试剂处理墨绿B染料模拟废水.研究了电压、pH值、温度、空气流量、支持电解质的浓度等因素对染料脱色率的影响.结果表明,pH值越低,温度越高,处理效果越好,气流量的改变对于处理效果影响不大.室温时处理浓度为50mg·L-1的活性染料墨绿B,在实验电压为11V,中性条件下,无水硫酸钠的浓度为20g·L-1,通入空气流量为60L·min-1时,处理60min,色度去除率达到95%左右.55℃时,电解30min色度去除率就达到96%,60min时达到100%.     

普鲁士兰修饰碳黑微电极同时微分伏安法测定多巴胺和抗坏血酸

将含有1.0%普鲁士蓝的碳黑与固体石蜡按2.5∶1(质量比)混合后装入φ0.2mm的石英毛细管中,在其上端插入一铂丝并抛光后即制成普鲁士蓝修饰碳黑微电极.对多巴胺(DA)及抗坏血酸(VC)在此电极上的电化学行为及应用此电极测定两组分的最佳条件进行了研究,在定量测定中采用二次微分线性扫描伏安法.在最佳条件下,DA与VC的峰电流(i″p)分别与各自的浓度保持如下线性关系DA为4.0×10-6～8.0×10-4mol·L-1,VC为6.0×10-5～1.0×10-3mol·L-1;检出限(3σ)依次为2.0×10-6mol·L-1及1.0×10-5mol·L-1.应用此方法分析了3种含DA及VC的混合溶液,测得结果的相对标准偏差(n=8)依次小于2.0%及3.0%,回收率范围依次为96.5%～101.0%及95.0%～102.5%.     

Investigation of the Cu-Zr-Y oxides activity in the carbon black catalytic oxidation by differential thermal analysis and temperature programmed reduction

Different copper/zirconium-yttrium catalysts have been tested in carbon black oxidation reaction. Supported mainly on differential thermal analysis and temperature programmed reduction, two different mechanisms have been proposed to explain the catalytic results. In the absence of copper, it has been shown that Zr³⁺ ions and associated anionic vacancies are responsible to the catalytic enhancement observed in the mixed oxides, oxygen species being activated on these sites. Among mixed zirconia-yttria solids, ZrO₂-5 mol%Y₂O₃ is the most active catalyst. Copper impregnation on these oxides leads to the formation of different copper species. Small particles of CuO in low interaction with the support, induce a catalytic improvement due to the highest reducibility of these species. Moreover, in order to be more efficient, CuO species should have some interactions with the support, since impregnated samples are more active than the simple mechanical mixtures.     

Effects of pressure and solvent on the diffusion of aromatic compounds through polymers

The diffusion of six azo and five anthraquinone derivatives through nylon 6, poly(ethylene terephthalate) and secondary cellulose acetate films were studied under high hydrostatic pressures of up to 3000 bar and at temperatures 80–130 °C, by analyzing the diffusion profiles yielded in a stacked multiple film, placed in the solution of the diffusant. It was found that the diffusion coefficient,D, of the diffusant decreased with increasing pressure, giving a linear relationship between InD and the pressure, the slope of which gave the activation volume for the diffusion,V . It was revealedV increased linearly with increasing intrinsic molecular volume of the diffusant,V _w , the slopes being different between the azo and the anthraquinone derivatives. The ratio ofV toV _w (V /V _w ) ranged from 0.13 to 0.93, depending in a sensitive manner on the degree of swelling of the polymer matrix which in turn was varied by the solvent. The overall results could be explained in accordance with the formulation,V _{f, local} +V =V _w , whereV _{f, local} represents the free volume contribution. It was proposed thatV _w is increased by solvation when the solvent is good for the diffusant.     

Spectral studies on the interaction of Amido black 10B with DNA in the presence of cetyltrimethylammonium bromide

The interaction of Amido black 10B (AB) with DNA in basic medium was studied in the presence of cetyltrimethylammonium bromide (CTMAB) based on the measurements of resonance light scattering (RLS), UV–vis, CD spectra, and RLS imaging. The interaction has been proved to give a ternary complex of CTMAB–DNA–AB in Britton–Robinson buffer of pH 11.55, which exhibits strong negative Cotton effect at 233.3 nm and 642.8 nm, and strong RLS signals characterized at 469 nm. Experiments showed that the enhanced RLS intensities (ΔI_RLS) against the mixture of AB and CTMAB are proportional to the concentration of fish sperm DNA (fsDNA) and calf thymus DNA (ctDNA), respectively over the range of 0.03–1.0 and 0.05–1.5 μg ml⁻¹, with the limits of determination (3σ) of 7.3 ng ml⁻¹ for fsDNA and 7.0 ng ml⁻¹ for ctDNA.     

Eu<Superscript>3+</Superscript>-fluorescence properties in nano-crystallized SnO<Subscript>2</Subscript>-SiO<Subscript>2</Subscript> glass-ceramics

Fluorescence and spectral hole burning properties of Eu³⁺ ions were studied in nanocrystals-precipitated SnO₂-SiO₂ glasses. The glasses were prepared to contain various amount of Eu₂O₃ using the sol-gel method, in which SnO₂ nanocrystals were precipitated by heating in air. In the glasses containing Eu₂O₃ less than 1%, the Eu³⁺ ions were preferentially doped in the SnO₂ nanocrystals and their fluorescence intensities were enhanced by the energy transfer due to the recombination of electrons and holes excited in SnO₂ crystals. The SnO₂ nanocrystals-precipitated glasses exhibited the persistent spectral holes with the depth of ∼25% of the total fluorescence intensities of the Eu³⁺ ions. With the increasing Eu₂O₃ concentration, the amount of SnO₂ nanocrystals decreased and the Sn⁴⁺ ions formed the random glass structure together with the silica network. This structure change induced the fluorescence intensities and the hole depth to decrease.