Authors:Mei-E Yue, Qiaoyan Lin, Jie Xu and Ting-Fu Jiang
A rapid, simple, and sensitive method has been developed for the analysis of pyrethroid herbicides in fruits by using headspace in-tube microextraction (HS-ITME) coupled with reverse-flow micellar electrokinetic capillary chromatography (RF-MECC). In the newly developed method, by placing a capillary filled with background electrolyte (BGE) of RF-MECC in the HS above the sample solution, the pyrethroid herbicides were extracted into the acceptor phase in the capillary. After extraction, electrophoresis of the extracts in the capillary was carried out. The influence of some essential BGE components such as sodium dodecyl sulfate (SDS) and organic modifiers concentrations was investigated. Extraction parameters were also systematically investigated, including the extraction temperature, extraction time, salt concentration, and volume of the sample solution. Under the optimized conditions, enrichment factors for three pyrethroids were 309, 133, and 288, respectively. The proposed method provided a good linearity, low limits of detection (below 1.00 ng/mL), and good repeatability of the extractions (relative standard deviations [RSDs] below 7.83%, n = 6). The fruit samples were analyzed by the proposed method, and the obtained results indicated that the proposed method provides acceptable recoveries and precisions.
Authors:Bing Xue, Kai Jia, Jie Xu, Na Liu, Ping Liu, Chongfu Xu and Yongxin Li
An efficient and novel method to prepare KNO3/NaY solid base catalysts was developed. High selectivity for phenetole along with high conversion of phenol was obtained in the vapor phase O-alkylation of phenol with diethyl carbonate over KNO3 modified NaY zeolite. Experimental results showed that a large number of basic sites on KNO3/NaY were generated mainly during catalytic evaluation, which was responsible for the outstanding catalytic performance. Furthermore, the excess KNO3 loadings might lead to the blockage of the pores in the NaY zeolite and decrease the catalytic activity.
Authors:Longshan Zhao, Qing Li, Yan Cui, Jie Wang, Shanshan Xu, Xiaohui Chen and Kaishun Bi
The thermal decomposition of a new antibiotic agent, cefuroxime lysine, was investigated by thermogravimetry analysis/derivative thermogravimetry and differential scanning calorimetry (DSC) methods in anoxic and oxidative environments. The influence of heating rates (including 5, 10, 15, and 20 °C/min) on the thermal behavior of cefuroxime lysine was revealed. By the methods of Kissinger and Flynn–Wall–Ozawa, the thermal kinetic parameters of activation energy and pre-exponential factor for the exothermic processes under non-isothermal conditions were calculated using the analysis of corresponding DSC curves.
Authors:Jiangang Yu, Jianguo Xu, Zhiqun Yu, Yi Jin, Jie Li and Yanwen Lv
A continuous-flow reactor (Corning G1 reactor) was hereby introduced for Fischer indole synthesis of 3-methylindole by reaction of phenyl hydrazines and propylaldehyde. Stoichiometric Lewis acid, ZnCl2, was supplied as catalyst as well as remover of NH3 which generated during the indole ring formation. Ionic liquid ([EMIM][BF4]) was employed as solvent according to its high-temperature tolerance and good product distribution. After a straightforward extraction process, 3-methylindole could be obtained in a 95.3% yield (96.0% purity) under optimized conditions. Ionic liquid (IL) was then recovered by another extraction process, and the recovered IL acted nearly as efficiently as new IL for this Fischer indole reaction.
Authors:Huang Wei, Jie Xiong, Xiaojun Chen, Xiaoling Gao, Yunshu Xu and Yibei Fu
Polyether-urethane samples were irradiated at the dose range from 10 to 2000 kGy by 2 MeV electron beams. Volatile species
from the polymer degradation were analyzed quantitatively and qualitatively with GC/MS. Thermal properties and micro-phase
separation of the samples were examined by TG and the morphology was studied by TEM and SEM. The results show that the irradiated
polyether-polyurethane evolves CO2, H2, CH4 and C2H6, etc. The thermal stabilities between the hard and soft segments in the irradiated samples are different. At high doses,
the phase separation in the sample is predominant and the hard segment of sample is more stable. The dose rate affects the
soft segment of the irradiated sample much more.
Authors:Kang-Zhen Xu, Xian-Gang Zuo, Hang Zhang, Biao Yan, Jie Huang, Hai-Xia Ma, Bo-Zhou Wang and Feng-Qi Zhao
A new high-energy organic potassium salt, 1-amino-1-hydrazino-2,2-dinitroethylene potassium salt [K(AHDNE)], was synthesized by reacting of 1-amino-1-hydrazino-2,2-dinitroethylene (AHDNE) and potassium hydroxide in methanol aqueous solution. The thermal behavior of K(AHDNE) was studied using DSC and TG/DTG methods and can be divided into three obvious exothermic decomposition processes. The decomposition enthalpy, apparent activation energy and pre-exponential factor of the first decomposition process were −2662.5 J g−1, 185.2 kJ mol−1 and 1019.63 s−1, respectively. The critical temperature of thermal explosion of K(AHDNE) is 171.38 °C. The specific heat capacity of K(AHDNE) was determined using a micro-DSC method, and the molar heat capacity is 208.57 J mol−1 K−1 at 298.15 K. Adiabatic time-to-explosion of K(AHDNE) was also calculated. K(AHDNE) presents higher thermal stability than AHDNE.