Short columns with molecularly imprinted monolithic stationary phases for rapid separation of diastereomers and enantiomers

Three molecularly imprinted monolithic columns with different length but almost identical column volume had been prepared. It was observed that the separation factors of diastereomers and enantiomers were almost unaffected by column length. However, the short column with dimension of 38 mm x 8 mm W. showed much lower resistance to flow rate so that it could be operated at much higher flow rates. By combining stepwise gradient elution with elevated flow rate, the diastereomers of cinchonine and cinchonidine and the enantiomers of Cbz-DL-Trp and Fmoc-DL-Trp were successfully separated within 3 min on the short column with dimension of 38 mm. x 8 mm i.d.. Based on the above results, a cinchonine imprinted monolithic disk with dimension of 10 mm x 16 mm W. was further developed. The SEM image and the pore size distribution profile showed that large flow-through pores are present on the prepared monolith, which allowed mobile phase to flow through the disk with very low resistance. Chromatographic performances on the monolithic disk were almost unchanged compared with the long columns. A rapid separation of cinchonine and cinchonidine was achieved in 2.5 min at the flow rate of 9.0 ml/min. Furthermore, it was observed that there was almost no effect of the flow rate on the dynamic binding capacity at high flow rates. In addition, the effect of the loading concentration of analytes on the dynamic binding capacity, namely adsorption isotherm, was also investigated. A non-linear adsorption isotherm of cinchonine was observed on the molecularly imprinted monolith with cinchonine as template, which might be a main reason to result in the peak tailing of template molecule. (C) 2004 Elsevier B.V. All rights reserved.

Optimizing the formation of in vitro sponge primmorphs from the Chinese sponge Stylotella agminata (Ridley)

The establishment and optimization of in vitro primmorph formation from a Chinese sponge, Stylotella agminata (Ridley), collected from the South China Sea, were investigated. Our aims were to identify the key factors affecting primmorph formation in this species and to optimize the technique for developing an in vitro primmorph culture system. The size of dissociated cells from S. agminata is relatively small, in the range between 5 and 10 mum. Round-shaped primmorphs of less than 100 gm were formed 3 days after transferring the dissociated cells into seawater containing Ca2+ and Mg2+. The effect of various cell dissociation conditions, inoculum. cell density, concentration of antibiotics, pH, and temperature was further investigated upon the formation of primmorphs. The time required for primmorph formation, primmorph size distribution, and the proliferating capability were microscopically documented. Healthy sponge S. agminata, inoculum. cell density and culture temperature play a critical role for the successful formation of primmorphs and that the microbial contamination will have to be controlled. (C) 2002 Elsevier Science B.V. All rights reserved.

Preparation of highly active Pt/C cathode electrocatalysts for DMFCs by an improved aqueous impregnation method

An improved aqueous impregnation method was used to prepare 40 wt% Pt/C electrocatalysts. TEM analysis of the samples showed that the Pt particles impregnated for a short time have a very narrow size distribution in the range of 1-4 nm with an average size of 2.6 nm. UV-vis spectroscopy measurements verified that the redox reaction between PtCl62- and formaldehyde took place with a slow rate at ambient temperature via a two-step reaction path, where PtCl42- serves as an intermediate. The use of the short-time-impregnated 40 wt% Pt/C as cathode electrocatalysts in direct methanol fuel cells yields better performance than that of commercial 40 wt% Pt/C electrocatalyst. Experimental evidence provides clues for the fundamental understanding of elementary steps of the redox reactions, which helps in guiding the design and preparation of highly dispersed Pt catalyst for fuel cells.

The synthesis of nanostructured W2C on ultrahigh surface area carbon materials via carbothermal hydrogen reduction

Nanostructured tungsten carbides were synthesized, for the first time, with a size distribution of 5-12 nm on ultrahigh surface area carbon material, by carbothermal hydrogen reduction (CHR) at 850degreesC and metal Ni promoted CHR at 650 degreesC.

Preparation and characterization of multiwalled carbon nanotube-supported platinum for cathode catalysts of direct methanol fuel cells

Multiwalled carbon nanotube-supported Pt (Pt/MWNT) nanocomposites were prepared by both the aqueous solution reduction of a Pt salt (HCHO reduction) and the reduction of a Pt ion salt in ethylene glycol solution. For comparison, a Pt/XC-72 nanocomposite was also prepared by the EG method. The Pt/MWNT catalyst prepared by the EG method has a high and homogeneous dispersion of spherical Pt metal particles with a narrow particle-size distribution. TEM images show that the Pt particle size is in the range of 2-5 nm with a peak at 2.6 nm, which is consistent with 2.5 nm obtained from the XRD broadening calculation. Surface chemical modifications of MWNTs and water content in EG solvent are found to be the key factors in depositing Pt particles on MWNTs. In the case of the direct methanol fuel cell (DMFC) test, the Pt/MWNT catalyst prepared by EG reduction is slightly superior to the catalyst prepared by aqueous reduction and displays significantly higher performance than the Pt/XC-72 catalyst. These differences in catalytic performance between the MWNT-supported or the carbon black XC-72-supported catalysts are attributed to a greater dispersion of the supported Pt particles when the EG method is used, in contrast to aqueous HCHO reduction and to possible unique structural and higher electrical properties when contrasting MWNTs to carbon black XC-72 as a support.

Preparation of uniform calcium alginate gel beads by membrane emulsification coupled with internal gelation

With the objective of making calcium alginate gel beads with small and uniform size, membrane emulsification coupled with internal gelation was proposed. Spherical gel beads with mean size of about 50 mum, and even smaller ones in water, and with narrow size distribution were successfully obtained. Experimental studies focusing mainly on the effect of process parameters on bead properties were performed. The size of the beads was mainly dependent on the diameter of the membrane pores. High transmembrane pressure made for large gel beads with wide size distribution. Low sodium alginate concentration produced nonspherical beads, whereas a high concentration was unsuitable for the production of small beads with narrow distribution. Thus 1.5% w/v was enough. A high surfactant concentration favored the formation of small beads, but the adverse effect on mass transfer should be considered in this novel process. (C) 2002 Wiley Periodicals, Inc.

Degradation of aquatic humic material by ultraviolet light

Natural humic water was treated with ultraviolet (UV) light and UV + hydrogen peroxide . The effects on the dissolved organic carbon content (DOC), the UV-absorbance at 254 nm (UV-abs.), the molecular size distribution, pH, and mutagenic activity were monitored, and the identity and concentrations of the most abundant gas chromatographable organic degradation products were determined. The DOC content and the UV-abs. of the water decreased substantially during treatment with. The decreases were dependent on the time of irradiation (UV dose) as well as on the H2O2 dose applied. The humus macromolecules were degraded to smaller fragments during irradiation. At higher UV doses, however, part of the dissolved organic matter (DOM) was found to precipitate, probably as a result of polymerization. Oxalic acid, acetic acid, malonic acid, and n-butanoic acid were the most abundant degradation products detected. These acids were found to account for up to 20% and 80% of the DOM in UV- and waters, respectively. No mutagenic activity was generated by the UV irradiation or the treatment. It is further concluded that the substantial mutagenic activity formed during chlorination of humic waters cannot be decreased by using UV irradiation as a pretreatment step.

黑龙江省安达市草地碱化后土壤物理性状变化

调查了安达市盐碱地生物资源环境研究中心试验区羊草Leymus chinensis地土壤物理性状,包括土壤硬度、含水量、饱和导水率、粒径分布、剖面特征和土壤温度等。阐明土地碱化对土壤物理性质的影响,为安达市以及松嫩平原生态环境的修复和土地资源的永续利用提供科学依据。同时,讨论了地下水化学成分和土壤冻融变化对碱化的可能影响,认为在没有植被覆盖的条件下,冻融变化会加剧土壤的碱化程度。

黄河流域泥沙矿物成分与分布规律

黄河及其干支流经常产生高含沙水流,泥沙中矿物的成分及含量是影响高含沙水流性质的主导因素,粘土矿物颗粒含量对高含沙水流流变性质的影响,远大于颗粒粒径大小对流变性质的影响,粘土颗粒和阳离子之间的相互作用对高含沙水流的流变性质也有非常大的影响。通过对黄河及其支流地区12个地点进行采样分析,得出黄河及其支流地区泥沙基本来源于同一地区,次生矿物是在长期的、相同的环境条件作用下形成的。根据泥沙样本的粒径分布曲线和矿物成分及含量,建立了黄河及其支流泥沙粘土、非粘土矿物含量与中值粒径之间的关系,能够更方便、快捷、廉价地估算黄河及其支流粘土矿物的含量。

Modelling raindrop impact and splash erosion processes within a spatial cell: a stochastic approach

A new approach is proposed to simulate splash erosion on local soil surfaces. Without the effect of wind and other raindrops, the impact of free-falling raindrops was considered as an independent event from the stochastic viewpoint. The erosivity of a single raindrop depending on its kinetic energy was computed by an empirical relationship in which the kinetic energy was expressed as a power function of the equivalent diameter of the raindrop. An empirical linear function combining the kinetic energy and soil shear strength was used to estimate the impacted amount of soil particles by a single raindrop. Considering an ideal local soil surface with size of I m x I m, the expected number of received free-failing raindrops with different diameters per unit time was described by the combination of the raindrop size distribution function and the terminal velocity of raindrops. The total splash amount was seen as the sum of the impact amount by all raindrops in the rainfall event. The total splash amount per unit time was subdivided into three different components, including net splash amount, single impact amount and re-detachment amount. The re-detachment amount was obtained by a spatial geometric probability derived using the Poisson function in which overlapped impacted areas were considered. The net splash amount was defined as the mass of soil particles collected outside the splash dish. It was estimated by another spatial geometric probability in which the average splashed distance related to the median grain size of soil and effects of other impacted soil particles and other free-falling raindrops were considered. Splash experiments in artificial rainfall were carried out to validate the availability and accuracy of the model. Our simulated results suggested that the net splash amount and re-detachment amount were small parts of the total splash amount. Their proportions were 0.15% and 2.6%, respectively. The comparison of simulated data with measured data showed that this model could be applied to simulate the soil-splash process successfully and needed information of the rainfall intensity and original soil properties including initial bulk intensity, water content, median grain size and some empirical constants related to the soil surface shear strength, the raindrop size distribution function and the average splashed distance. Copyright (c) 2007 John Wiley & Sons, Ltd.

Observation of Nucleation and Growth of CdS Nanocrystals in a Two-phase System

The nucleation and growth kinetics of CdS nanocrystals in a two-phase synthesis system have been investigated. It was found that the nucleation process is quite lengthy and overlapped with the growth process; nevertheless, as formed nanocrystals show extremely narrow size distribution owing to the unique heterogeneous reacting environment and Ostwald ripening growth. The nucleation and growth kinetics of the nanocrystals were also influenced strongly by the monomer concentration, capping agent concentration, and solvent polarity. It was also found that a high monomer concentration, a low capping agent concentration, and low solvent polarity lead to a higher maximum nucleus concentration and nanocrystal concentration, while high polarity solvents are favorable for the formation of nanocrystals with narrower size distribution and higher photoluminescence quantum yield.

Vulcanization of polybutadiene latex induced by Co-60 gamma radiation

Polybutadiene latex (PBL) vulcanization induced by Co-60 radiation and the influence of dose on crosslinking were investigated. Morphology and particle size distribution were examined by AFM and a particle size analyzer. The casting films were characterized for their swelling and mechanical properties as a function of dose.

Phase Behavior and self-assembly of poly[N-vinylformamide-co-(acrylic acid)] copolymers under highly acidic conditions

Copolymers of N-vinylformamide and acrylic acid were synthesized by conventional aqueous free-radical polymerization. The phase behavior of the copolymer solutions was investigated through the addition of hydrochloric acid and the variation of the temperature. With a moderate content of N-vinylformamide, the copolymers showed complex phase behaviors. Under low-acidity conditions, a suspending liquid was formed, whereas under high-acidity conditions, the random copolymers could assemble into round nanoparticles with a broad particle size distribution.

A simple selenium source to synthesize CdSe via the two-phase thermal approach

A novel selenium source was developed to synthesize the size-controlled CdSe nanocrystals with relatively narrow size distribution successfully in a two-phase thermal approach. A highly reactive and aqueous soluble selenium source was provided by the reduction of selenite, and in this route the size of the nanocrystals can be adjusted by the reaction temperature and time. The size, crystalline structure and optical characteristics of these nanocrystals were investigated by transmission electron microscopy, X-ray powder diffraction, X-ray photoelectron spectroscopy, UV-vis spectroscopy, and photoluminescence spectroscopy. The influence factors for this approach were also discussed.

Carbon-supported Pd nanocatalyst modified by non-metal phosphorus for the oxygen reduction reaction

A carbon-supported palladium catalyst modified by non-metal phosphorus(PdP/C) has been developed as an oxygen reduction catalyst for direct methanol fuel cells.The PdP/C catalyst was prepared by the sodium hypophosphite reduction method. The as-prepared Pd nanoparticles have a narrow size distribution with an average diameter of 2 nm. Energy dispersive X-ray analysis (EDX), X-ray photoelectron spectroscopy (XPS), and X-ray diffraction (XRD) results indicate that P enters into the crystal lattice of Pd and forms an alloy.