硫代乙酰胺体系电沉积法制备CdS纳米膜

The film of surface active agents spread out on the surface of the electrolyte of Thioacetamide and cadmium chloride. CdS nanofilm was deposited at the interface of surface active agents and electrolyt by the method of electrodeposition. The optimal conditions on which the nanofilm was prepared of the least crystals and uniform particles could be attained via analytical results of L₁₆(4⁵) orthogonal experiments. The optimal conditions: castor oil/hexadecanoll 0.06 mL·cm^-2，CdCl₂/CH₃CSNH₂ 4 mmol·L^-1, cell voltage 5 V, electrodeposition temperature 15 ℃. The effects on the grain size of temperature, surface-active agent, electrodyte concentration, cell voltage and pH become smaller in the series. If the temperature was high, the movement of molecules of surface-active agent and electrodyte would be faster, thus the preparation of the film would be difficult. The grain size of thinfilm varied with the surface-active agents, however, when the amount of surface-active agents reached a certain value, the grain size would remain unchanged. The higher the electrodyte concentration, the larger the grain size of nanofilm. The surface forms were changed at the same time. If the pH of the electrodyte was higher or lower, nanofilm could not be prepared successfully, thus the pH range should be is 3～6. SEM image of the nanofilm shows the occurance of dendrite. The sucessful preparation of nanofilm is closely related to the nature of surface activre agent due to the nanofilm growth mechanism.     

Selection of Conditions for the Dynamic Sorption Preconcentration of a 1,1-Dimethylhydrazine Derivative (4-Nitrobenzaldehyde N,N-Dimethylhydrazone) on Hydrophobized Silica

The type of mass transfer in the sorption of 4-nitrobenzaldehyde N,N-dimethylhydrazone (BDH) on silica chemically modified with hexadecyl groups was determined using the linear model of sorption dynamics, and distribution and mass transfer coefficients of hydrazone were calculated. Optimal conditions of the dynamic sorption preconcentration and desorption of BDH and its subsequent determination by reversed-phase high-performance liquid chromatography were proposed. The detection limit of the compound for preconcentration from a sample of 100 mL was 1 g/L.     

含羟基芳基或氨基芳基的磷酰胺酯衍生物的合成

采用均相反应的方法合成了6个含羟基芳基或氨基芳基的磷酰胺酯衍生物:[(ClCH_2CH_2)_2NP(O)(OPh)(XArY)](X:O,NH;Y:m或p-OH或NH_2).用元素分析、红外光谱、氢核磁共振谱及质谱证实了它们的组成及结构.     

微乳液体系中过硫酸钾氧化碘离子的动力学研究

分别在不同盐浓度的自由水和不同液滴尺寸的微乳液中测量了过硫酸钾氧化碘 离子的化学反应速率常数，获得微乳液不核中水的活度，探讨了水的活度及体系中 离子强度与反应速率的关系，发现当表面活性剂与水的摩尔比R≤20时，水的活度 随微反应器尺寸减小而快速下降。     

DL－苹果酸－丙酮－BrO~3^-－Mn^2^+－H~2SO~4化学振荡 反应诱导期的新特征 及其动力学研究

在前文研究工作的基础上,较详细地研究了DL-苹果酸(以下简称DL-MA)、丙酮(以下简称Act)参与下的新型化学振荡反应及各种影响因素,对各主要参与反应物质在诱导期中的作用、起振原因、诱导期的新特征和可能反应机理进行了较为深入的研究,分别获得DL-MA,KBrO~3,MnSO~4的浓度对诱导期影响的拟合方程。以及诱导期的表观活化参数为E~I~N=68.50kJ·mol^-^1。     

On-Line Sorption–Chromatographic Determination of Phenols with Amperometric Detection

Conditions of the preconcentration of phenol on a microcolumn filled with MN-200 hypercrosslinked polystyrene were determined using the linear sorption dynamics model. Conditions of the on-line determination of phenol and its chloro derivatives by reversed-phase high-performance liquid chromatography with amperometric detection were optimized. The detection limit of phenol and chlorophenols for preconcentration from 30 mL of a sample was 3 and 15 ng/L, respectively. The proposed procedure was used for the determination of phenols in tap and river water.     

超临界CO2法制备头孢唑啉钠脂质体

采用超临界CO2(scCO2)流体代替有机溶剂一步法制备了头孢唑啉钠药物载体脂质体. 研究了该脂质体的尺寸、稳定性和药物的包封率. 结果表明, 脂质体的尺寸和稳定性依赖于制备压力, 脂质体对头孢唑啉钠的包封率与乙醇和脂浓度有关, 采用超临界CO2法制备脂质体的药物包封率比采用薄膜分散法(Bangham method)制备的包封率高.     

高效液相色谱-串联质谱法结合多糖衍生物手性固定相拆分氰戊菊酯

建立了以多糖衍生物为手性固定相的高效液相色谱-串联质谱(HPLC-MS/MS)直接拆分氰戊菊酯对映体的方法。在反相液相色谱条件下,考察了手性固定相的种类、流动相组成、柱温、流速对氰戊菊酯4个立体异构体分离的影响。同时,利用热力学方法对氰戊菊酯的立体异构体与固定相之间的色谱保留和分离的热力学机理进行了探讨。结果表明:采用Lux Cellulose-3(纤维素-三(4-甲基苯甲酸酯))手性色谱柱,在以流动相为乙腈-水(5 mmol/L甲酸铵)=(55:45,V:V)流速0.4 mL/min,柱温30℃的条件下,可在14 mins内实现氰戊菊酯4个立体异构体的基线分离。拓展了HPLC-MS/MS在菊酯类手性农药对映体分离及检测上的应用。     

Unusual cleavage of phenacyl-substituted benzimidazolium salts. Synthesis of 1,4-diarylimidazoles

The action of ammonium acetate in acetic acid on 1-alkyl(aralkyl)-3-phenacylbenzimidazolium bromides leads, in addition to the formation of a new imidazole ring, to cleavage of the benzimidazole fragment of the molecule at the 1,2 bond to give 1-alkyl(aralkyl)aminoaryl-4-arylimidazoles. 1,2-Dimethyl-3-(p-nitrophenacyl)benzimidazolium bromide is converted under similar conditions to the corresponding 2-methylimidazole. 4,4-Dimethyl-2,2-bis(p-nitrophenyl)-1,1-dipyrrolo[1,2-a]benzimidazole was isolated as a side product of this reaction.Translated from Khimiya Geterotsiklicheskikh Soedinenii, No. 3, pp. 388–392, March, 1982.     

2,2'-二乙炔基-1,1'-联萘为模板构筑的新的环芳化合物的合成及其光学性质

基于2,2'-二取代的联萘衍生物在手性构型上高度稳定的特点,分别以光学活性的(R)-和(S)-2,2'-二乙炔基-1,1'-联萘为模板,设计了2个有趣的拓扑环芳分子四联萘笼状对映异构体(R,R,R,R)-2和(S,S,S,S)-2.其合成路线涉及保护基的控制导入、苯连接桥的链接、保护基的脱去以及偶合成环反应4个步骤.用MS,IR,UV-Vis,1HNMR,13CNMR和元素分析等技术对其进行了表征,并比较了其光学性质.研究结果表明,采用这种模板合成方法能够有效地获得具有单一手性的目标化合物.镜像特征的圆二色(CD)谱和比旋光度[α]D的测定结果清楚地反映了它们的对映异构关系.