N-(1-异丙基-2-羧基-4-甲基二环[2.2.2]-5-辛烯-3-羰基)-N′-芳基(硫)脲的合成

在无溶剂绿色化学条件下,将α-萜品烯-马来酸酐加成物(1)与取代苯(硫)脲发生N-酰化反应,合成了4个N-(1-异丙基-2-羧基-4-甲基二环[2.2.2]-5-辛烯-3-羰基)-N′-芳基(硫)脲化合物(3a~3d),并由IR、UV-Vis、MS、1HNMR、13C NMR和元素分析确认了目标产物的结构。生物活性测试表明,其中3个化合物(3a、3b和3c)具有植物激素作用。     

Ordered nickel oxide nanowire arrays and their optical absorption properties

Ordered NiO nanowire arrays embedded in anodic alumina membranes have been prepared by using an electrochemical deposition method. After annealing at 300 °C, the NiO nanowire arrays were characterized using SEM, TEM, SAED, and XRD. SEM and TEM observations reveal that these nanowires are dense, continuous and arranged roughly parallel to one another. XRD and SAED analysis together indicate that these NiO nanowires crystallize with a polycrystalline structure. The optical absorption band gap of NiO nanowire arrays is 3.74 eV, and no obvious blue shift or red shift with respect of that of the bulk NiO can be observed.     

两组份互穿网络聚合物的合成研究

以蓖麻油聚氨酯和聚醚聚氨酯的不同重量比与光敏剂、催化剂、稀释剂、促进剂所组成的多相体系为反应物,分别在紫外光照射和加热的条件下合成网络Ⅰ和网络Ⅱ的互穿网络聚合物(IPN)。改变网络Ⅱ聚醚聚氨酯中各组份的摩尔比制得系列样品。红外光谱,应力-应变曲线和动态力学性能测定发现,样品的力学性能与两组份重量比和网络Ⅱ中不同组成都存在着一定关系。这些结果,为该体系IPN的合成和应用提供了一定依据。     

反相液相色谱中固定相和流动相对柱相比的贡献

依据柱相比的热力学定义和反相液相色谱中溶质的计量置换保留理论(the stoichiometric dispheement heory of solute for retention，SDT-R)，对反相液相色谱中固定相和流动相性质、温度对柱相比的影响进行了研究。结果表明：固定相的种类和配基的疏水性对柱相比影响较大，而流动相中有机溶剂的种类，特别是脂肪酸作为置换剂时，对柱相比的影响更大，而柱相比受温度的影响较小。此外，通过用27种小分子溶质对柱相比的测定，其logI和Z良好的线性关系，进一步证明柱相比是一个与溶质性质无关的常数。     

Dependence of Elution Curve and Adsorption Isotherms of Insulin on composition of Mobile Phase of Frontal Analysis in Reversed Phase Liquid Chromatography

With frontal analysis(FA),the dependence of adsorption isotherms of insulin on the composition of mobile phase in reversed phase liquid chromatography (RPLC) has been investigated,This is also a good example to employ the stoichiometric displacement theory (SDT) for ivestigating solute adsorption in physical chemistry.Six kinds of mobile phase in RPLC were employed to study the effects on the elution curves and adsorption isotherms of insulin.the key points of this paper are:(1) the stability of insulin due to delay time after preparing,the organic solvent concentration,the kind and the concentration of ion-pairing agent in mobile phase were found to affect both elution curve and adsorption isotherm very seriously.(2)To obtain a valid and comparable result,the composition of the mobile phase employed in FA must be as same as possible to that in usual RPLC of either analytical scale or preparative purpose.(3)Langmuir Equation and the SDT were employed to imitate these obtained adsorption isotherms.The expression for solute adsorption from solution of the SDT was found to have a better elucidation to the insulin adsorption from mobile phase in RPLC.     

Carbon nanohorns grown from ruthenium nanoparticles

A nanoscale ruthenium/gold bimetallic cluster of clusters has been used as a molecular precursor to produce pure ruthenium nanoparticles (seeds) as catalysts for the growth of carbon nanohorns (CNHs).     

Studies on the refolding of the reduced-denatured insulin with size exclusion chromatography

The refolding of the reduced-denatured insulin from bovine pancreas was investigated with the size exclusion chromatography (SEC). It was shown that the reduced-denatured insulin originally denatured with 7.0 mol L^?1 guanidine hydrochloride (GuHCI) or 8.0 mol L^?1 urea could not be refolded with a non-oxidized mobile phase. Although the oxidized and reduced glutathione (GSSG and GSH) were employed in the oxidized mobile phase, the reduced-denatured insulin still could not be renatured. However, in the presence of 2.0 mol L^t-1 urea in the oxidized mobile phase employed, the reduced-denatured insulin can be refolded with SEC, and the aggregation of denatured insulin can be diminished by urea. In addition, the disulfide exchange of reduced-denatured insulin also can be accelerated with GSSG/GSH in the oxidized mobile phase. The three disulfide bridges of insulin were formed correctly and the reduced-unfolded insulin can be renatured completely. The results were further tested with reversed-phase liquid chromatography (RPLC) and hydrophobic interaction chromatography (HIC).     

Hydrogen bonding networks controllable by the substitution position of tetrathiafulvalene on the pyridine ring

Because of the effect of pyridine on the substituent position on the TTF group, TTF derivatives exhibit different assembly structures at the interface, which will be of great significance to the construction of functional nanostructures from the molecular design point of view.     

比值光谱导数法同时测定铝合金中铁,铜,锌

用比值光谱－导数分光光度法，在ｐＨ５．５缓冲溶液中，利用金属－２－（５－溴－２－吡啶偶氮）－５－二乙氨基酚（５－Ｂｒ－ＰＡＤＡＰ）－ＯＰ三元络合物显色体系，对混合物中铁，铜，锌三组分进行了同时测定。合成试样５次测定回收率在９７．３％－１０４．４％之间。应用于铝合金中铁，铜，锌的测定，各６次测定的ＲＳＤ分别为３．６６％，１．３８％，２．０３％。     

液相色谱中一个新的表征参数Z：Ⅱ.反相液相色谱中小分子极性溶质体系

反相高效液相色谱（ＲＰＬＣ）中小分子极性溶质的极性是可以用液相色谱中溶质计量置换保留模型中的Ｚ值（１ｍｏｌ溶质被固定相吸附时，在固定相与溶质子间释放出置换剂的ｍｏｌ数）来表征的，其大小可用带有该极性端基的同系物的Ｚ值对碳原子数线性作图的截距求得。这些检性基的Ｚ测量定值与疏水性片段指数１ｇｆ间有极好的线性关系。依此关系还可测出一些用其他实验方法无法测得的某些基团的１ｇｆ值。