Preparation and characterization of superfine ammonium perchlorate (AP) crystals through ceramic membrane anti-solvent crystallization

In this paper, a novel ceramic membrane anti-solvent crystallization (CMASC) method was proposed for the safe and rapid preparation ammonium perchlorate (AP) crystals, in which the acetone and ethyl acetate were chosen as solvent and anti-solvent, respectively. Comparing with the conventional liquid anti-solvent crystallization (LASC), CMASC which successfully introduces ceramic membrane with regular pore structure to the LASC as feeding medium, is favorable to control the rate of feeding rate and, therefore, to obtain size and morphology controllable AP. Several kinds of micro-sized AP particles with different morphology were obtained including polyhedral-like, quadrate-like to rod-like. The effect of processing parameters on the crystal size and shape of AP crystals such as volume ratio of anti-solvent to solvent, feeding pressure and crystallization temperature were investigated. It is found that higher volume ratio of anti-solvent to solvent, higher feeding pressure and higher temperature result in smaller particle size. Scaning electron microscopy (SEM) and X-ray diffraction (XRD) were used to characterize the resulting AP crystals. The nucleation and growth kinetic of the resulting AP crystals were also discussed.     

Controlled chemical co-precipitation and solid phase synthesis,microstructure and photoluminescence of La3PO7:Eu3+ phosphors

Eu³⁺-doped oxy-phosphate (La₃PO₇:Eu³⁺) with monoclinic phase has been synthesized via solid phase and co-precipitation methods. The products present various regular morphologies after high temperature thermal treatment, such as bulk with holes, leaf-like flake, nano-rod and so on. All the phosphors exhibit the characteristic fluorescence of Eu ion, the electric dipole transition ⁵D₀→⁷F₂ of Eu³⁺ ions is dominant indicating that the sites of Eu³⁺ ions in La₃PO₇ have no the inversion center. Furthermore, the intensity of ⁵D₀→⁷F₂ increases due to the introducing of surfactant and increasing of the calcination temperature.     

Interfacial structure of oxidized inner pores in precursor-derived Si–C–N ceramics

Inner pore channels were commonly found in precursor-derived Si–C–N ceramics. After annealing in air at 1420 °C, their oxidation structures were investigated by analytical TEM. A carbon-rich ring was frequently observed under the silica layer inside the pore channels, which consisted of graphite-like clusters in size of 20–30 nm. Origin of such interfacial structure is due to the excessive free-carbon in the amorphous Si–C–N matrix that had survived the oxidation process. This graphitic interface could further improve the oxidation resistance of the SiO₂ over-layer. This novel interfacial structure was also found by annealing in N₂, reaffirming the effect of composition of Si–C–N matrix.     

Spinnablity and structure characterization of mullite fibers via sol–gel-ceramic route

Viscosity and rheology behaviors of the mullite sols prepared from aqueous solution of aluminum nitrate, aluminum isopropoxide and tetraethylorthosilicate has been investigated. Rheological measurement suggested that mullite sols exhibited good spinniabilty when the evaporation of the solvent is allowed during sol–gel process. Spinnable sols showed shear-thinning flow behavior with high viscosity to the time of gelation. By adjusting temperature, the gelation degree and viscosity of the sol could be stabilized at a certain value and the sol–gel transition could be transferred to the spinning line of a laboratory dry-spinning apparatus. Continuous mullite fibers were obtained from such sols using sol gel dry-spinning method. The final ceramic fibers had smooth surfaces with an average diameter of 50 μm. Structure evolution of mullite ceramic fibers were characterized by MAS NMR and specific surface area analyses.     

Novel Designs for Centrifugal Countercurrent chromatography: V. Comparative Studies on Performance of Various Column Configurations

The conventional toroidal coil in centrifugal countercurrent chromatography has a low level of stationary phase retention, since a half of each helical turn is entirely occupied by the mobile phase. In order to cope with this problem, several new column designs including zigzag, saw-tooth and figure-8 patterns have been introduced and their performance was compared in terms of retention of the stationary phase (Sf), peak resolution (Rs), theoretical plate number (N) and column pressures. Overall results of experiments indicate that the figure-8 column yields the highest Rs when the lower phase is used as the mobile phase. Since the column pressure of all these new columns are much lower than that in the traditional toroidal coil column, the separation efficiency can be improved using a long separation column without a risk of column damage by high back pressure.     

Method development and inter-laboratory comparison about the determination of titanium from titanium dioxide nanoparticles in tissues by inductively coupled plasma mass spectrometry

Nanosized titanium dioxide (TiO₂) is one of the most interesting and valuable nanomaterials for the construction industry but also in health care applications, food, and consumer goods, e.g., cosmetics. Therefore, the properties associated with this material are described in detail. Despite its widespread use, the analytical determination and characterization of nanosized metal oxides is not as straightforward as the comparatively easy-to-detect metallic nanoparticles (e.g., silver or gold). This study presents the method development and the results of the determination of tissue titanium (Ti) levels after treatment of rats with the nanosized TiO₂. Total Ti levels were chosen to evaluate the presence and distribution of TiO₂ nanoparticles. A procedure consisting of incubation with a mixture of nitric acid (HNO₃) and hydrofluoric acid (HF), and heating was developed to digest tissues and TiO₂ nanomaterials in order to determine the total Ti content by inductively coupled plasma mass spectrometry (ICPMS). For the inter-laboratory comparison, altogether four laboratories analyzed the same samples upon digestion using the available ICPMS equipment. A major premise for any toxicokinetic study is the possibility to detect the chemical under investigation in biological samples (tissues). So, the study has to be performed with a dose high enough to allow for subsequent tissue level measurement of the chemical under investigation. On the other hand, dose of the chemical applied should not induce over toxicity in the animal as this may affect its absorption, distribution, metabolism, and excretion. To determine a non-toxic TiO₂ dosage, an acute toxicity study in rats was performed, and the organs obtained were evaluated for the presence of Ti by ICPMS. Despite the differences in methodology and independent of the sample preparation and the ICPMS equipment used, the results obtained for samples with Ti concentrations >4 μg Ti/g tissue agreed well.

QSAR Studies on the COX-2 Inhibition by 3,4-Diarylcycloxazolones Based on MEDV Descriptor

Selective inhibition of cyclooxygenase-2 (COX-2) might avoid the side effects of current available nonsteroidal antiinflammatory drugs while retaining their therapeutic efficacy. A novel variable selection and modeling method based on prediction is developed to construct the quantitative structure-activity relationships (QSAR) between the molecular electronegativity distance vector (MEDV) based on 13 atomic types and the biological activities of a set of selective cyclooxygenase-2 inhibitory molecules, 3,4-diarylcycloxazolones (DAA) plus indomethacin,naproxen, and celecoxib. Using multiple linear regression, a 5-variable linear model is developed with the calibrated correlation coefficient of 0.9271 and root mean square error of 0.17 in modeling stage and the validated correlation coefficient of 0.9030 and root mean square error of 0.20 in leave-one-out validation step, respectively. To further test the predictive ability of the model, 20 DAA compounds are picked up to construct a training set which is used to build a QSAR model and then the model is employed to predict the biological activities of the balance compounds. The predicted correlation coefficient and root mean square error are 0.9332 and 0.19, respectively.     

负反馈诱发神经电振荡的反常现象的复杂动力学

传统观念认为,负反馈容易使系统达到稳定平衡点而正反馈容易引起振荡.本研究基于神经元理论模型,提出了负反馈可以诱发稳定平衡点、也就是静息、变为振荡、也就是放电的新观点.在Hopf分岔点附近,作用在静息上的一次足够大的负向脉冲电流的抑制性刺激,能够引起一个动作电位及随后的衰减振荡的后电位;而能够在后电位上诱发出动作电位的负脉冲电流强度阈值也是衰减振荡的.在模型中,引入具有时滞($\tau$)的负反馈来模拟抑制性自突触,一个动作电位诱发的负反馈自突触电流会作用到比动作电位延迟$\tau$的后电位上.随时滞增加,能够诱发出放电的负反馈增益强度阈值呈现出具有衰减振荡特点的类似多重相干共振的特性,衰减振荡的周期与电流阈值曲线的周期以及分岔点附近的放电周期相关.另外,负反馈还能诱发出放电与静息共存的复杂行为.本研究的结果不仅揭示了负反馈的新的反常调控作用,还有助于理解在现实神经系统中存在的慢抑制性自突触的潜在功能.      

A microbial synthesis of R and S-9-hydroxy-(E)-2-decenoic acid(9-HDA), a queen honeybee pheromone

(R,E)-9-hydroxy-2-decenoic acid (9-HDA) its (S,E)- isomer have been prepared by using an organic-microbial approach.     

丙烯酸β-羟基γ-(邻乙酰氧基苯甲酰氧基)丙酯的合成及其聚合

<正> 将近来发现具有抗血小板凝聚效应的阿斯匹林进行高分子化的研究迄今尚少报告,我们曾合成了酯基上带有邻-乙酰氧苯甲酰氧基的丙烯酸酯类;甲基丙烯酸β-(乙酰水杨酰氧)乙酯;甲基丙烯酸β-(乙酰水杨酰氧)丙酯及丙烯酸β-(乙酰水杨酰氧)乙酯,本文合成了在酯基上兼有羟基和邻-乙酰氧基苯甲酰氧基的丙烯酸酯;甲基丙烯酸