An experimental and theoretical approach to the molecular structure of 3‐{[4‐(3‐Methyl‐3‐phenyl‐cyclobutyl)‐thiazol‐2‐yl]‐hydrazono}‐1,3‐dihydro‐ indol‐2‐one

The title molecule, 3‐{[4‐(3‐methyl‐3‐phenyl‐cyclobutyl)‐thiazol‐2‐yl]‐hydrazono}‐1,3‐dihydro‐indol‐2‐one (C₂₂H₂₀N₄O₁S₁), was prepared and characterized by ¹H NMR, ¹³C NMR, IR, UV–visible, and single‐crystal X‐ray diffraction. The compound crystallizes in the monoclinic space group P21 with a = 8.3401(5), b = 5.6976(3), c = 20.8155(14) Å, and β = 95.144(5)°. Molecular geometry from X‐ray experiment and vibrational frequencies of the title compound in the ground state has been calculated using the Hartree–Fock with 6‐31G(d, p) and density functional method (B3LYP) with 6‐31G(d, p) and 6‐311G(d, p) basis sets, and compared with the experimental data. The calculated results show that optimized geometries can well reproduce the crystal structural parameters, and the theoretical vibrational frequencies values show good agreement with experimental data. Density functional theory calculations of the title compound and thermodynamic properties were performed at B3LYP/6‐31G(d, p) level of theory. © 2011 Wiley Periodicals, Inc. Int J Quantum Chem, 2012     

Ionic Liquids for and by Analytical Spectroscopy

Abstract

In this mini‐review we highlight two aspects of ionic liquids that to date have either no or limited studies. They are (1) exploitation of unique features of ionic liquids to develop novel spectroscopic methods and (2) development of novel spectroscopic methods, for the sensitive and accurate determination of thermal physical properties of ionic liquids. In the first category, we will describe several novel methods which were developed utilizing unique properties of ionic liquids for measurements which are not possible otherwise. They include the sensitive and accurate method to determine enantiomeric compositions of a variety of pharmaceutical products with different size, shape, and functional groups. This method is based on the use of a chiral IL which serves both as a solvent and also as a chiral selector. Ionic liquids have also been successfully used to substantially enhance the sensitivity of thermal lens measurements. In the second category, we will describe recent development in which transient grating technique and thermal lens technique have been successfully used for the sensitive, accurate, nondestructive determination of thermal physical properties of ILs.     

Simultaneous Determination of Atrazine and Chlorpyrifos in Pesticide Formulations,in Soils and Waters by Derivative Spectrophotometry and Ratio Spectra Derivative

Abstract

A new method is described to analyse a binary mixture of atrazine and chlorpyrifos, using first-derivative spectrophotometry for atrazine and first derivative of the ratio spectra for chlorpyrifos. The procedure does not require any separation step. Calibration graphs were linear up to 15 μg.mL^?1 of atrazine and to 10 μg.mL^?1 of chlorpyrifos. The method has been applied to determine both compounds in pesticide formulations, in soils and waters.     

3-(4,5-二苄硫基-1,3-二硫杂环戊烯-2-亚基)萘吡喃酮的合成、性质及量子化学计算

设计合成了一种新的具有D-π-A体系的有机分子:3-(4,5-二苄硫基-1,3-二硫杂环戊烯-2-亚基)萘吡喃酮,通过UV-vis,1H NMR,13C NMR,TOFMS和IR确定了其结构.初步研究了该化合物的电子光谱、荧光光谱和热稳定性.运用Gaussian 03量子化学程序包,采用密度泛函(DFT)B3PW91的方法优化了其基态几何结构,得到的几何参数与实验结果吻合得很好.研究结果表明,体系中存在着分子内的电荷转移,有较好的荧光性质,为寻找新的发光材料具有一定的实际意义.     

近红外光谱法测定5-羟基色氨酸的含量

本文利用近红外光谱法建立了5-羟基色氨酸的偏最小二乘(PLS)定量模型。采用相关数法选择波段以及二阶导数、Norris derivative平滑滤波进行数据预处理,所建校正模型的R为0.99907,RMSEC为0.0638,RMSEP为0.0675。经验证模型的预测性能良好,为5-HTP的快速测定提供了一种方法。     

基于角度度量法的混纺纤维定量检测

采用“基于角度度量的多变量回归方法”对维纶和腈纶混纺纤维各组分含量进行检测,并与直接用偏最小二乘法（PLS）对混和纤维的预测结果作对比。实验结果显示,PLS法对维纶和腈纶预测值与实际值的线性相关系数r均为0．9457,标准偏差为6．0906,均方根误差为6．9948。角度度量法对维纶预测值与实际值的线性相关系数r为0．9990,标准偏差为0．8929,均方根误差为2．1896;对腈纶预测值与实际值的线性相关系数r为0．9928,标准偏差为2．1896,均方根误差为3．9493。实验证明,角度度量法比PLS法更能准确表达定量关系,角度度量法可以显著降低分析操作对环境的要求,满足了近红外光谱在混纺纤维定量分析上的要求。     

荧光素衍生物在TiO_2胶体中的光物理性质研究

测定了以荧光素为光敏剂的电子给体-受体二元化合物荧光素蒽醌甲酯（FL- AQ）及模型化合物荧光素丁酯（FL4）在溶液中和在二氧化钛（TiO_2）胶体中的吸 收光谱、荧光光谱、荧光寿命等。发现荧光素蒽醌甲酯与荧光素丁酯均可通过酚羟 基较好地吸附在TiO_2胶体上。从吸收光谱可得,FL4与TiO_2形成表面络合物的表 观结合常数（K_(app)）大约为3590 mol~(-1)·L,结合率（α）为0.86;FL-AQ与 TiO_2形成表面络合物的K_(app)大约为3060 mol~(-1)·L,α为0.84。同时通过 ESR光谱讨论了光诱导电子注入机制。     

傅里叶变换红外光谱和气相色谱-质谱法快速检测鼠药

用傅里叶变换红外光谱(FT-IR)差谱技术和气相色谱．质谱(GC/MS)全扫描法及特征离子监测技术，建立了毒鼠强和氟乙酰胺的标准质谱图库。利用有机溶剂直接萃取与FT-IR和GC/MS的结合，建立了混合组分原形物中毒鼠强和氟乙酰胺的快速检测方法。对7份实际样品的鉴定获得满意的结果。建立的方法为侦破案件提供了快速、灵敏、准确、有效的分析手段。     

meso-5,10,15,20-四[4-(N-吡咯烷基)苯基]卟啉的合成及对牛血清白蛋白的作用

基于卟啉对癌细胞的特殊亲和作用和吡咯烷化合物的抗肿瘤及抗癌活性,设计并合成了具有吡咯烷结构的新型卟啉化合物--meso-5,10,15,20-四[4-(N-吡咯烷基)苯基]卟啉(TBPPH₂),利用荧光光度法和紫外-可见分光光度法研究了TBPPH₂与牛血清白蛋白(BSA)的相互作用.实验发现,TBPPH₂利用疏水作用力进入BSA的疏水性腔,与BSA形成配合物并引起BSA的静态荧光猝灭.在TBPPH₂与BSA的相互作用过程中,TBPPH₂与BSA以摩尔比1∶1牢固结合,TBPPH₂与BSA分子中色氨酸间的最近距离r=2.4nm.反应平衡常数K_A=2.51×10⁴L/mol,反应熵变ΔS=84.18J/(mol·K),TBPPH₂与BSA的结合常数K_B=5.13×10⁵L/mol.研究结果表明,吡咯烷基卟啉可能成为一类新型的抗肿瘤及抗病毒药物.     

单壁纳米碳管的纯化研究

A purification method to remove the metal catalysts and impurity carbon materials from arc-discharge-grown single-walled carbon nanotubes (SWCNTs) has been developed. Microporous membrane and the oxidation in the air for the crude SWCNTs were used to eliminate the coexisting metal catalysts nanoparticles，carbon nanoparticles and amorphous carbon. Then we used the high resolution transmission electron microscopy (HRTEM) to characterize the crude SWCNTs prepared by arc-discharge method and the purified SWCNTs. The Raman spectra and the thermogravimetric analysis (TGA) were also utilized to analyze the approach of our purification for SWCNTs. With this method the SWCNTs with the purity more than 95% could be obtained.