凝胶渗透色谱净化-气相色谱法测定茶叶中30种有机氯及菊酯类农药残留量

茶叶样品(1.00g)用水5 mL湿润后加入50mL乙腈高速匀浆提取3min。混合物滤入已盛有固体氯化钠2 g的具塞量筒中,取上清液20.0mL于45℃蒸发至近干,加入乙酸乙酯环己烷(1+1)混合溶剂10.0mL溶解残渣后进行凝胶渗透色谱(GPC)净化。流动相为上述混合溶剂,流量为4.7mL·min~(-1)。收集9～20min时间段的流出液,在45℃蒸至近干,加正己烷定容为5.0mL,供气相色谱分析。采用Rxi-5MS石英毛细管柱进行分离和电子捕获检测器进行检测,所测农药的线性范围为0.02～0.50mg·L~(-1)。检出限(3S/N)在1×10~(-4)～2×10~(-3)mg·kg~(-1)之间。试验测得方法的回收率在83.2%～114.6%之间,测定值的相对标准偏差(n=5)在0.9%～4.8%之间。     

接枝聚苯乙烯/多壁碳纳米管纳米复合材料制备及合成机理

通过原位悬浮聚合的方法, 以过氧化苯甲酰(BPO)做引发剂, 制备了聚苯乙烯/多壁碳纳米管(MWNT-g-PS)纳米复合材料, 复合材料在水和乙醇中均表现出良好的分散性及稳定性. 通过高倍透射电镜(HRTEM)、场发射扫描电镜(FESEM)分析, 多壁碳纳米管上包覆有1～3 nm的聚苯乙烯膜, 并分布有半径从几十纳米到几百纳米不等的聚苯乙烯微球. 通过傅立叶变换红外光谱(FTIR)、拉曼光谱(Raman spectroscopy)、X光电子能谱(XPS)和热重分析(TGA)对复合材料进行分析, 结果表明, 自由基将多壁碳纳米管表面π键打开, 形成一种新的自由基, 引发聚苯乙烯的自由基聚合, 形成了接枝聚苯乙烯/多壁碳纳米管纳米复合材料.     

2-羟基-1-萘醛缩氨基脲的抗菌活性及其与牛血清白蛋白的结合作用研究

采用滤纸片法和打孔法2种抗菌试验方法,考察2-羟基-1-萘醛缩氨基脲（NAHSEM）对金黄色葡萄球菌、大肠杆菌、枯草杆菌的抗菌活性的结果表明,NAHSEM对3种细菌具有较强的抗菌活性。荧光光谱法研究了NAHSEM与牛血清白蛋白（BSA）的结合作用表明,这种结合行为使BSA的内源荧光猝灭。通过猝灭常数、结合常数和结合位点...     

An in situ oxidation route to fabricate graphene nanoplate-metal oxide composites

We report our studies on an improved soft chemical route to directly fabricate graphene nanoplate-metal oxide (Ag₂O, Co₃O₄, Cu₂O and ZnO) composites from the in situ oxidation of graphene nanoplates. By virtue of H⁺ from hydrolysis of the metal nitrate aqueous solution and NO₃⁻, only a small amount of functional groups were introduced, acting as anchor sites and consequently forming the graphene nanoplate-metal oxide composites. The main advantages of this approach are that it does not require cumbersome oxidation of graphite in advance and no need to reduce the composites due to the lower oxidation degree. The microstructures of as-obtained metal oxides on graphene nanoplates can be dramatically controlled by changing the reaction parameters, opening up the possibility for processing the optical and electrochemical properties of the graphene-based nanocomposites.     

气相色谱法测定DNT废酸、废水中的甲苯及硝基甲苯等含量

研究气相色谱在测定废水、废酸中甲苯、硝基甲苯含量方面的应用.根据相关标准及废酸、废水处理的实际情况确定最佳的实验条件,废水样12次测定结果的相对标准偏差小于0.5％,加标回收率为98.31％.该法测定结果精确度高,适合DNT废酸、废水处理的分析监控.     

Matrix-assisted pulsed laser evaporation of polyimide thin films and the XPS study

Compared with the traditional thin film techniques, the matrix-assisted pulsed laser evaporation (MAPLE) technique has many advantages in the deposition of polymer and organic thin films. It has a wide range of applications in many fields, such as non-linear optics, luminescent devices, electronics, various sensors. We have successfully deposited polyimide thin films by using the MAPLE technique. These films were characterized with XPS. The XPS spectra showed that the single-photon effect is ob-vious at low laser fluence and the chemical bonds will be broken, resulting in decomposition of the films. Contrarily, the single-photon effect will decrease and the multi-photon effect and the photothermal effect will increase at high laser fluence, resulting in the protection of the structure of the polyimide thin films and the obvious decrease in decomposition. High laser fluence is more suitable for the deposition of polymer and organic thin films than low laser fluence.     

Catalytic Reaction of Aryldiazoacetates with Indole and Its Derivatives:Profound Effect of N‐1 Substitutent on the Reaction Pathways

The reaction of indole and its derivatives with aryldiazoacetates has been studied in the presence of copper and rhodium catalysts. The electronic property of N-1 substitutent showed significant effect on the reaction pathways. The electron-donating group favored the formation of the β-alkylation products, while the electron-withdrawing group favored the formation of the cyclopropane products. A reaction mechanism was proposed based on the experimental data and previous research results. The structure of aryl group in diazo compounds also affected the yield of the β-alkylation products or the cyclopropane products.     

Photoluminescence and Electroluminescence of Organic Light Emitting Diodes Based on Tris‐(8‐quinolinolato) Aluminum Nanoparticles

利用共沉淀方法制备出平均粒径为20nm的有机物8-羟基喹啉铝纳米粒子,8-羟基喹啉铝纳米粒子呈球形且粒度不随老化时间的增加而改变。本文研究了8-羟基喹啉铝纳米粒子的光致发光及基于8-羟基喹啉铝纳米粒子制作的电致发光器件的电致发光特性。8-羟基喹啉铝形成纳米粒子后,其光致发光及电致发光发射光谱的谱峰均出现蓝移。随着驱动电压的增加,器件中8-羟基喹啉铝纳米粒子的发射峰逐渐红移。在驱动电压为16伏时,8-羟基喹啉铝纳米粒子器件的最大亮度达600cd/m²,电流密度为150mA/cm^-2时,器件的发光效率为0.19cd/A。基于8-羟基喹啉铝纳米粒子器件的发射光谱证实了AlQ₃纳米粒子具有量子尺寸效应的存在,这为有机纳米电致发光器件的研究开辟了一条新的研究路线,同时也为那些传统的有机材料如有机分子晶体的基础研究探索出新的研究方向。     

一种新颖的二维4f-3d-5d多金属-异烟酸配合物的合成、晶体结构和磁性研究

通过水热方法合成了一种新颖的异金属金属-异烟酸无机-有机杂化体[Zn0.5(H2O)]{(Hg2Cl5)[Er(C6NO2H4)3(H2O)2]}(HgCl2)·0.5CH3OH·0.5H2O (1)并对其进行了单晶X-射线衍射结构表征。该化合物是首例4f-3d-5d多金属-异烟酸配合物。化合物1属于单斜晶系C2/c空间群,每个单胞中有8个分子,晶体学参数为：a = 34.165(4) Å,b = 9.4692(8) Å,c = 24.575(3) Å,β = 115.090(5)°,V = 7200(1) Å3,C18.50H21Cl7ErHg3N3O10Zn0.50,Mr = 1495.25,Dc = 2.759 g/cm3,T = 293(2) K,μ(MoKα) = 15.954 mm-1,F(000) = 5400, R1/wR2 = 0.0561/0.0909,共有6468个独立衍射点,其中[I > 2σ(I)]的有3157个。该化合物具有新颖的二维{(Hg2Cl5)[Er(C6NO2H4)3(H2O)2]}层状结构,由Hg2Cl5–连接[Er(C6NO2H4)3(H2O)2]链形成。该二维层和氯化汞及结晶水之间通过氢键形成三维结构,甲醇分子和水合锌离子位于该三维结构的空隙中。对化合物1的磁性测试显示该化合物具有反铁磁作用。     

氟烷基叠氮化合物和缺电子烯烃反应的研究

本论文研究了氟烷基叠氮化合物和缺电子烯烃的1,3-偶极反应, 合成了一系列含氟烷基三唑啉和氟烷基吡唑啉类化合物, 并提出了一个通过开环和以重氮化合物为中间体的反应机理.