Synthesis of 4‐(5‐aryl‐1,3,4‐oxadiazol‐2‐yl)phenyl‐hydrazine derivatives from 3‐(4‐hydrazinocarbonyl‐phenyl)sydnones

The synthesis of potential fluorescent active 4‐(5‐aryl‐1,3,4‐oxadiazol‐2‐yl)phenylhydrazine derivatives was accomplished in three steps. The key step was the dehydration cyclization of 1,2‐diacylhydrazines to form the 1,3,4‐oxadiazole ring by use of acetic anhydride/perchloric acid mixture as the dehydrating agent. The sydnone moiety served as the masked hydrazines, which could be demasked by HCl for further application. © 2007 Wiley Periodicals, Inc. Heteroatom Chem 18:438–442, 2007; Published online in Wiley InterScience ( www.interscience.wiley.com ). DOI 10.1002/hc.20318     

Size of Micelles Determined by Static Fluorescence Quenching

We developed a new method to measure the average aggregation number of large rod-like micelles using static fluorescence self-quenching of a solubilized fluorophore. The method is based on the increase of self-quenching of micelle-solubilized pyrene through excimer formation. We consider the effect of random distribution of pyrene in micelles and the micellar size distribution. The measured average aggregation <n> _M is based on a new M-weighted raging similar to our exponential-weighted averaging in the transient decay method. We apply this method to study the effect of a large concentration of salt on the average aggregation behavior of sodium dodecyl sulfate (SDS) and cetyle tetraammonium bromide (CTAB). The sizes increase with increasing ionic concentrations. For SDS, we used the thermodynamic model developed by Missel et al. to calculate < n > _M which we compare with experimental results.     

Characterizations of iron-rich clay modified electrodes and their applications in optical recognition

Optical recognition was studied with modified electrodes based on iron-rich clays. According to energy-dispersive X-ray spectroscopy (EDX), several clay minerals including montmorillonite K10 (mont. K10) contain a lot of iron. Cyclic voltammetry suggested that electrochemically active iron species exist in most iron-rich clays and are likely to reside at different sites. The associated electrochemical activity is strongly pH-dependent and photosensitive. Under UV irradiation (λ ≤ 420 nm), these iron species were activated, and a pronounced photocurrent resulted. When these electrodes were flow-injected with 2-pyridylcarboxylic acids (λ_ab,max = 260 nm), the originally monotonic photocurrent could be modulated into a more recognizable a.c. pattern and the 260 nm optical signal became distinguishable. The photoresponse was highly reproducible, and the response time (t₉₀) was less than 10s.     

高效离子排斥色谱法测定饮料中的糖精钠

提出了一种用高效离子排斥色谱法测定饮料中糖精钠的新方法。以ＩｏｎＰａｃ ＩＣＥ－ＡＳ ６柱为分离柱，０．１０ ｍｍｏｌ／ＬＨ２ＳＯ４＋甲醇（９＋１）为淋洗液，２０２ｎｍ波长下紫外检测。在１－１００ｍｇ／Ｌ范围内，糖精钠的含量与峰面积呈 良好线性关系。检出限为０．６０ｎｇ，灵敏度优于以往采用离子交换色谱－电导检测法的结果。在实验条件下，饮料 中常见有机酸以及其它人工合成甜味剂等均不产生干扰。方法用于饮料中糖精钠的测定，加标回收率为９８％～ １０５％。此外还比较了电导检测、紫外检测和经化学抑制系统后紫外检测等三种检测方式对测定灵敏度的影响。     

Comparison of hydrothermal,hydrotropic and organosolv pretreatment for improving the enzymatic digestibility of bamboo

Pretreatment is the crucial step to disrupt the recalcitrant structure of lignocellulosic biomass for improving the enzymatic hydrolysis efficiency. Typically, hydrothermal, organosolv and hydrotropic pretreatments are environmentally benign and effective methods. In this work, effects of hydrothermal, organosolv and hydrotropic pretreatments on improving enzymatic hydrolysis of bamboo were comprehensively compared. Hydrotropic pretreatment was more effective in removal lignin and xylose from bamboo fiber cell wall. However, the surface coverage by lignin and extractives were dramatically displaced during organosolv pretreatment as investigation by X-ray photoelectron spectroscopy. After pretreatments, the crystallinity of cellulose in pretreated substrates has a significant reduction, and pores were exposed on fiber surface. The residual content of acetyl and phenolic groups in hydrotropic pretreated substrates is lower than organosolv pretreated substrates. In order to deeply assess the delignification of pretreatments, the isolated lignins obtaining from pretreatments process were characterized by Fourier transform infrared spectroscopy also. It was revealed that hydrotropic lignin contained more phenolic hydroxyl group and syringyl units than organosolv lignin. Compared to hydrothermal and organosolv pretreatment, cellulase adsorption capacity of pretreated substrates was notably improved by hydrotropic pretreatment, which indicating the better enzyme accessibility of cellulose. Eventually, the maximum glucose yield was obtained from hydrotropic pretreated substrates.     

Water-annealing regulated protein-based magnetic nanofiber materials: tuning silk structure and properties to enhance cell response under magnetic fields

In this study, flexible silk fibroin protein and biocompatible barium hexaferrite (BaM) nanoparticles were combined and electrospun into nanofibers, and their physical properties could be tuned through the mixing ratios and a water annealing process. Structural analysis indicates that the protein structure of the materials is fully controllable by the annealing process. The mechanical properties of the electrospun composites can be significantly improved by annealing, while the magnetic properties of barium hexaferrite are maintained in the composite. Notably, in the absence of a magnetic field, cell growth increased slightly with increasing BaM content. Application of an external magnetic field during in vitro cell biocompatibility study of the materials demonstrated significantly larger cell growth. We propose a mechanism to explain the effects of water annealing and magnetic field on cell growth. This study indicates that these composite electrospun fibers may be widely used in the biomedical field for controllable cell response through applying different external magnetic fields.     

A Universal Cassette-Based System for the Dissolution of Solid Targets

Cyclotron-based radionuclides production by using solid targets has become important in the last years due to the growing demand of radiometals, e.g., ⁶⁸Ga, ⁸⁹Zr, ^43/47Sc, and ^52/54Mn. This shifted the focus on solid target management, where the first fundamental step of the radiochemical processing is the target dissolution. Currently, this step is generally performed with commercial or home-made modules separated from the following purification/radiolabelling modules. The aim of this work is the realization of a flexible solid target dissolution system to be easily installed on commercial cassette-based synthesis modules. This would offer a complete target processing and radiopharmaceutical synthesis performable in a single module continuously. The presented solid target dissolution system concept relies on an open-bottomed vial positioned upon a target coin. In particular, the idea is to use the movement mechanism of a syringe pump to position the vial up and down on the target, and to exploit the heater/cooler reactor of the module as a target holder. All the steps can be remotely controlled and are incorporated in the cassette manifold together with the purification and radiolabelling steps. The performance of the device was tested by processing three different irradiated targets under different dissolution conditions.     

Improved Electrocatalytic Activity and Stability by Single Iridium Atoms on Iron-based Layered Double Hydroxides for Oxygen Evolution

Full understanding to the origin of the catalytic performance of a supported nanocatalyst from the points of view of both the active component and support is significant for the achievement of high performance. Herein, based on a model electrocatalyst of single-iridium-atom-doped iron (Fe)-based layered double hydroxides (LDH) for oxygen evolution reaction (OER), we reveal the first completed origin of the catalytic performance of such supported nanocatalysts. Specially, besides the activity enhancement of Ir sites by LDH support, the stability of surface Fe sites is enhanced by doped Ir sites: DFT calculation shows that the Ir sites can reduce the activity and enhance the stability of the nearby Fe sites; while further finite element simulations indicate, the stability enhancement of distant Fe sites could be attributed to the much low concentration of OER reactant (hydroxyl ions, OH⁻) around them induced by the much fast consumption of OH⁻ on highly active Ir sites. These new findings about the interaction between the main active components and supports are applicable in principle to other heterogeneous nanocatalysts and provide a completed understanding to the catalytic performance of heterogeneous nanocatalysts.     

Structure of Cytochromec and Its Platinum-modified Derivatives by Fourier Transform Infrared Spectroscopy

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