Precise lattice parameter measurements in CsCl-Br solid solutions between room temperature and 90°K by powder x-ray diffraction

Solid solutions of CsCl-Br in five different concentrations were prepared in sealed quartz tubes by heating the mixture to 1123°K for 6–8 hr and quenching to room temperature. X-ray diffractograms were taken at eight different temperatures between room temperature and 90°K for these solid solutions using the YPC50NM powder diffractometer and a continuous flow cryostat. The observed lattice parameters for each sample at each temperature obtained from the powder diffractograms were then extrapolated to give the true lattice parameters using the least square method with Nelson-Riley extrapolation scheme. The values of the true lattice parameters at each concentration and at each temperature were tabulated and the results discussed. It is shown that the lattice parameters vs temperature for some concentrations exhibit an anomalous behaviour. Contribution No. 691     

Synthesis and characterization of a novel nano-scale magnetic solid base catalyst involving a layered double hydroxide supported on a ferrite core

A nano-scale magnetic solid base catalyst MgAl-OH-LDH/MgFe₂O₄ (where LDH denotes layered double hydroxide) composed of MgAl-OH-LDH Brønsted base catalytic layers coated on MgFe₂O₄ spinel cores has been prepared. A magnetic precursor MgAl-CO₃-LDH/MgFe₂O₄ was prepared by a method involving separate nucleation and aging steps, and subsequently calcined to give a mixed metal oxide composite MgAl(O)/MgFe₂O₄ which was rehydrated to give MgAl-OH-LDH/MgFe₂O₄. The structure and magnetic properties of the nano-scale magnetic solid base MgAl-OH-LDH/MgFe₂O₄, together with those of the magnetic precursor MgAl-CO₃-LDH/MgFe₂O₄ and MgFe₂O₄ were characterized by XRD, XPS, low temperature N₂ adsorption and vibrating sample magnetometry (VSM). The MgAl-OH-LDH/MgFe₂O₄ composite possesses a mesoporous structure with pore size ranging from 2 to 20 nm with particle size mainly in the range 35-130 nm. The catalytic properties of MgAl-OH-LDH/MgFe₂O₄ were evaluated using the self-condensation of acetone at 273 K as a probe reaction. The results showed that the conversion of acetone to diacetone alcohol reached the thermodynamic equilibrium value of 23% at 273 K. The catalyst was easily recovered through application of an external magnetic field, and when the reclaimed catalyst was used in a second run for the same reaction, the reactivity remained unchanged.     

Immobilized polysiloxanes as stationary phases for high-performance liquid chromatography and solid phase extraction

Polysiloxanes immobilized onto the surfaces of porous silica particles have proven to be good stationary phases for the separation of multiresidues of pesticides and their metabolic/degradation products by reversed-phase high-performance liquid chromatography (RP-HPLC). Similar materials have proven effective for pre-concentration and clean-up procedures using solid phase extraction. The present paper describes the preparation and some applications of several of these packing materials.     

陈化温度和Fe/Zr配比对SO42-/Fe2O3-ZrO2固体超强酸结构与性能的影响

用低温陈化法制备了SO42 -/Fe2 O3 ZrO2 (简称SFZ)固体超强酸催化剂 ,用红外光谱 (IR)和X光衍射(XRD)对其结构进行了表征 ,并考察了它对合成癸二酸二正丁酯的催化性能 .IR谱显示 ,低温陈化的SFZ样品在10 70cm-1处吸收峰远强于常温陈化样品 .XRD分析则显示 ,在焙烧温度为 6 5 0℃、Fe/Zr为 2∶1时 ,低温陈化的样品出现了亚稳态的ZrO2 四方晶相 .该样品在催化酯化反应中使产率达 90 %以上 ,高于常温陈化样品的 30 % .研究结果表明 :在其他条件不变时 ,低温陈化所出现的亚稳态的ZrO2 四方晶相是表面酸性和催化活性增加的微观原因     

Reversible 5′-end biotinylation and affinity purification of synthetic RNA

A reversible biotinylation phosphoramidite was synthesized and incorporated onto the 5′-end of an oligoribonucleotide on a solid phase synthesizer. After cleavage and deprotection, the crude synthetic oligomer mixture was incubated with NeutrAvidin^® coated microspheres, and the failure sequences removed by washing with a buffer followed by treating the microspheres with tetrabutylammonium fluoride to give a high quality unmodified full-length oligoribonucleotide.     

A transport model for the evolution of urban systems

When comparing an urban system to an elasto-plastic lattice, an analogy to the solid state of matter can be exploited using the concepts of the band theory similarly. Thereafter, the population dynamics – in a region of certain stability in the state space and within appropriate energy bands – can be described in terms of Cellular Automata, with two mobile agents or pseudo particles: the inhabitant (representative of an average individual) and the recurson (representative of its multidimensional resources). As in the solid state, transition rules take the form of two coupled transport equations, comprising the terms equivalent to the generation-recombination and circulation processes. The first process can be compared to a predator–prey growth model, typical of Ecology; whereas the circulation process – composed of a drift component and a diffusion component – should be compared to the concentration-sprawl demographic balance seen in urban occupation and dynamics. Thus, it needs to be defined and determined an urban potential function, an equivalent population charge, mobility and diffusion parameters, as well as net growth factors. This analogy, discussed within the context of a case study for Great Mendoza, plausibly explains the varied growth rates of the political departments, as well as the principal urban trends for spatial occupation.     

傅里叶变换红外光谱固体制样技术

通过对溴化钾与纳米固体超强酸样品的比例进行了探讨 ,得出制样时溴化钾与样品比例范围为1∶ 0 .0 0 1— 1∶ 0 .0 2 9,其最佳比例范围为 1∶ 0 .0 0 98— 1∶ 0 .0 1 5 ,并且应用于其他固体样品的测定 ,结果基本一致。同时得出 ,固体样品的最少检测量为 2 .0× 1 0 -5g     

Studies on Solid State Reactions of Coordination Compounds（LXXI）──Solid State Reactions of o－Aminobenzoic Acid with Copper（Ⅱ） Acetate and Formate at Room Temperature

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Trace enrichment and HPLC analysis of polycyclic aromatic hydrocarbons in environmental samples,using solid phase extraction in connection with UV/VIS diode-array and fluorescence detection

Summary Both the separation of polycyclic aromatic hydrocarbons (PAH's) on tailor made HPLC phases, and their chromatographic enrichment and quantitative determination are of great interest. Because of the generally low concentrations of PAH's in the environment, and the low limiting values in German legislation for drinking water, methods for selective enrichment and sensitive detection are indispensable. On account of their relatively high amounts in soil, the determination of PAH's is valuable for the assessment of the potential danger to ground water by waste materials. These requirements can be fulfilled by used of solid phase extraction on enrichment columns, and fluorescence or UV/VIS diode array detection. For the detection of PAH's in the picogram range, the wavelengths for excitation and emission were time programmed over the chromatogram. With this feature, it is possible to detect all the individual compounds at the highest sensitivity, over the entire analysis.     

La传感器在测定铝液凝固过程中La活度研究

微量稀土加入铝或铝合金中，如果加入方法、数量、时间得当，可明显改善材料的多项性能．稀土对铝及铝合金的影响规律和作用机理，已取得了一些进展，但对稀土铝合金的热力学性质，尤其是溶解态稀土的研究少有报导［‘，2］．本工作采用L即．95C。。。。FZ。。多晶作为固体电解