A New Method for Separation of Hydrophobic Au Nanoparticles in the Reversal Micelle

In this article, a new method which not only can separate hydrophobic Au nanoparticles (NPs), but also obtain highly monodisperse NPs is discussed. A self‐made device of two same burettes, one of which was inserted into the other, was used for separating the nanoparticles by washing the reversal micelle. The effects of separation were characterized and analyzed by micrograph of transmission electron microscope (TEM), UV‐vis spectra, quartz crystal microbalance (QCM), and energy dispersive x‐ray analysis (EDX). It has been shown that, the smaller nanoparticles are, the easier they are to stay at the reversal micelle and the narrower the sizes are. This method can be applied to synthesize highly monodisperse Au NPs.     

A Mossbauer study of the magnetic coupling in iron phosphorous trisulfides

The polycrystalline sample of layered compound FePS_3 has been investigated by using M?ssbauer spectroscopy (12K to 300K), magnetic susceptibility measurements, x-ray diffraction and FTIR spectroscopy. The antiferromagnetic order exists below T_N=120.5±1K. The M?ssbauer spectra below T_N indicate that the magnetization axis is perpendicular to the layer of FePS_3, and the divalent iron cations are in their high spin configurations. By fitting the hyperfine field parameters near the Néel temperature, we obtain information on the nature of magnetic interactions in the material. The results show that the magnetic coupling can be treated by the two-dimensional Ising model, and it can be interpreted on the basis of a crystal-field effect.     

N,N-二(2-苯并咪唑亚甲基)甲胺高氯酸盐的晶体和电子结构

合成了三齿配体N,N-二(2-苯并咪唑亚甲基)甲胺(MN3)的高氯酸盐.对该化合物进行了元素分析、紫外和红外表征;采用X射线衍射方法测定了该化合物的晶体结构,依据晶体结构数据使用G98程序对配体(MN3)进行了量子化学计算.     

中药色谱指纹图谱组分保留时间漂移的校准

基于光谱相关色谱方法判断复杂中药色谱指纹图谱的组分相关性,实现同一中药样本在不同实验条件下所得的色谱指纹图谱的相同组分的色谱保留时间漂移的局部最小二乘校正,为合理评价指纹图谱的品质提供较为实用的工具。     

厚朴酚合成方法的改进研究

本实验中,将2,2＇-联苯二酚与1-溴丁烷经Williamson反应后,利用该反应产物溴化钠在酸性条件下与溴酸钠反应生成初生态的溴作为溴源,溴代反应得到5,5＇-二溴-2,2＇-二丁氧基联苯.中间产物5,5＇-二溴-2,2＇-二丁氧基联苯制成Grignard试剂后与烯丙基溴反应生成5,5＇-二烯丙基-2,2＇-二丁氧基...     

湿化学法合成纳米ZrB2粉末

本文利用ZrO2-B2O3-C体系中碳热还原的基本原理,分别使用正丙醇锆(Zr(OC3H7)4)、硼酸(H3BO3)和蔗糖(C12H22O11)为原料,采用溶胶-凝胶法合成了ZrB2纳米粉末。在实验设计过程中,首先使用化学修饰剂乙酰丙酮(acac)修饰Zr(OC3H7)4,目的是防止Zr(OC3H7)4的快速水解;其次,选用蔗糖作为碳源,是考虑到蔗糖热解时可以完全分解为碳,这样可以准确计算热解过程碳的生成量。结果表明:当起始原料nB/nZr=2.3、热解温度为1550℃时,通过溶胶-凝胶法可以成功合成单相ZrB2纳米粉末。分布均匀的颗粒形貌呈等轴状,平均尺寸约50 nm。     

FeBr_3-catalyzed dibromination of alkenes and alkynes

The dibromination of alkenes and alkynes with bromosuccinimide and sodium bromide catalyzed by FeBr₃ under mild conditions has been developed.The trans-dibromo compounds were exclusively obtained with excellent yields.     

高效液相色谱法同时测定香兰素与邻位香兰素

建立了同时测定香兰素和邻位香兰素的高效液相色谱法.考察了流动相组成、柱温等因素对分析效率的影响.在流动相为5% 乙酸-乙腈(60 :40,体积比),流速1.0 mL/min,柱温25 ℃的优化条件下,香兰素和邻位香兰素可在5 min内实现分离.测定结果表明,香兰素和邻位香兰素在10 ～240 mg/L范围内线性关系良好...     

茶叶中多元素的微波消解等离子体发射光谱法测定

采用密闭式微波消解系统处理茶叶样品,以电感耦合等离子体发射光谱法测定茶叶样品中铜、铁、锌、锰、钡和铝6种元素.分别从消解液的选择、用酸量及样品消解量等方面进行消解条件的优化,对测定钡、铝元素存在的干扰进行了讨论.各元素的检出限范围为0.15～0.65μg·g-1,回收率为98.6%～106%,精密度为0.8%～5.3%...