原子吸收光谱法测定柞蚕蛹中铜铁锌钙

柞蚕蛹又名茧蛹 ,具有一定的药用价值[1 ] ,民间一直把它当作一种高蛋白的风味佳品。其体内各种微量元素的含量测量则尚未见报道。本文利用马弗炉干法灰化前处理 ,火焰原子吸收光谱法测定其中铜、铁、锌和钙的含量。对同一产地的同批柞蚕蛹平行测定 7次 ,铜、铁、锌和钙元素的相对标准偏差分别为 5.2 %、4 .3%、2 .7%和 2 .1 % ,四元素的加标回收率分别在 96%～ 1 0 2 % ,95%～ 98% ,94 %～1 0 3%和 97%～ 1 0 4 %之间。该方法与测定同类食品所常用的混酸湿法消解[2 ,3] 相对照 ,结果一致 ,但本法成本低、对环境污染小、简便快速。1　试验部…     

环丙沙星荷移反应及荧光光谱性质研究

研究了环丙沙星（CPFX）与电子受体2，3－二氰－5，6－二氯－1，4对苯酯（DDQ）之间的荷移反应。实验结果表明：DDQ与CPFX的荷移反应需在丙酮－甲醇（1：4）介质中进行。两者于40℃水浴中恒温30min即可形成1：1络合物，其荧光发射较CPFX有显著的增强。在0．107．2mg/L浓度范围内，荧光强度与质量浓度呈良好线性关系；其检出限为0．1mg/L。本方法用于片剂中环丙沙星的含量测定，其回收率为96．6％－100．2％；标准偏差为1．3％－2．6％。     

四苯基卟啉锌[ZnTPP(H_2O)]的晶体结构及性质研究

用X射线衍射法确定了四苯基卟啉锌（Ⅱ）水合物ZnC44H28N4（H2O）的晶体结构。晶体属于单斜晶系，C2空间群，a=18903（4），b=9．672（2），c=13．379（3）A，β=134．92（3）°，V=1732（1）A3，Z=2，Dx=1．335g／cm3，Mr=696．13，μ（MoKa）＝0．764mm－1,F（000）=720。最终偏离因子R=0．055，Rw=0．050（1076、个I≥3σ（I）衍射点）。配合物分子中Zn（Ⅱ）离子落入卟啉空腔内与4个吡咯氮原子共平面，在垂直该平面上与H对H2O分子呈轴向配位，其分子结构呈四方锥型。用电子吸收光谱和1HNMR波港以及循环伏安法对其性质进行表征，并对其轴向配位反应的热力学性质进行研究。     

双外推法研究FeC_2O_4·2H_2O脱水过程的动力学机理

在Coats-Redfern积分式和Ozawa公式的基础上，采用双外推法对FeC_2O_4·2H_2O脱水过程的最可能机理进行了研究．结果表明其脱水过程分两步进行：第一步脱水过程为成核与生长过程，G（α）函数积分式为[-ln（1-α）]1／1.5；第二步脱水过程为二维扩散过程，G（α）式为（1-α）ln（1-α）＋α；同时求得相应的动力学参数．     

掺铂二氧化钛纤维光催化降解氯仿的研究

 TiO2纤维作为一种微米级光催化剂应用于废水处理时，不但克服了TiO2纳米颗粒不易分离回收的困难，而且对其进行贵金属掺杂，可使其光催化活性大大提高．用光还原沉积法制备了掺铂的二氧化钛纤维催化剂（Pt／TiO2（F）），并将其作为光催化剂用于光催化降解氯仿反应，考察了掺铂量、氧及pH值等条件对降解氯仿反应的影响，并与掺铂的二氧化钛颗催化剂粒（Pt／TiO2（G））的光催化活性进行了比较．结果表明，当掺铂量w（Pt）＝0．5％，催化剂用量为0．5g／L，预先溶氧至饱和状态，c0（CHCl3）＝1mmol／L，pH＝5，用300W中压汞灯光照120min时，Pt／TiO2（F）上氯仿的降解率可达98．44％，而Pt／TiO2（G）上氯仿的降解率仅为72．03％．     

铁(Ⅱ)-4(5-溴-2-噻唑偶氮)邻苯二酚-乳化剂OP三元胶束络合物的分光光度研究

1引言小（5一仅一2一喷吐偶氛）邻苯二酚（简称5－Br－TAPC）是笔者合成的新有机试剂，迄今未见文献报道。由于在TAPC的喷吐环上引入了助包团一Br，故与铁（I）形成的络合物的人．二红移，最佳显色酸度酸移，显色反应的灵敏度和选择性提高。利用该显色体系所建立的水中痕县铁的测定方法简便、快速、准确，取得了满意的结果．2实验团分2．且主要试剂和仪器铁标准溶液：10．00ms／L；5－Br－TAPC（自制）乙醇溶液：1．00X10‘mol／L；抗坏血酸（AR）水溶液（新鲜配制）：0，5％；硼砂（AR）缓冲溶液：0．05mol／L（PH9．2）；乳化…     

低温条件下羰基硫催化水解反应本征动力学研究

 采用自行设计和安装的微反－色谱联用装置，在50～70℃，n（H2O）／n（COS）＝60～550的条件下，以TGH为催化剂，对羰基硫催化水解反应本征动力学进行了研究．利用不同的目标函数，采用非线性Marquart法对实验数据进行回归，所建立的本征动力学方程式为r（COS）＝－dXd（W／f（COS））＝1．82·1014p（COS）p－0．5（H2O）exp－758008．374T．并对其反应机理进行了探讨．     

2,2’-(4-氯苯基)亚甲基双(3-羟基-5,5-二甲基-2-环己烯-1酮)的晶体结构

标题化合物C23H27O4Cl是由邻氯苯甲醛与5，5-二甲基-1，3-环己二酮在N，N-二甲基甲酰胺中反应而得。结构通过单晶X-射线衍射法测定，其晶体属于单斜晶系，空间群晶体结构用直接法解出，使用全矩阵最小二乘法对原子参数进行修正，最后的偏离因子为在晶体结构中，存在两个共轭的烯醇式结构。四个C－O健长分别为1．283（2），1．285（2），1．287（3）和1．298（2）     

钙钛矿型(La_(0.8)M_(0.2))MnO_3和(La_(0.8)Sr_(0.2))(Mn_(1-x)Fe_x)O_3的XRD和IR光谱的研究

合成了（La0.8M0.2）MnO3（M=Ca2+，Sr2+，Ba2+）和（La0.8Sr0.2）（Mn1-xFex）O3（x=0．1、0．2、0．3、0．4、0．5）两类氧化物，经XRD确认为钙铁矿型氧化物，应用FT－IR对其进行研究，对主要的红外特征振动υ（Mn-O）和δ（O-Mn-O）进行分析表征。这类化合物的υ（Mn-O）和δ（O-Mn-O）的FT－IR特征吸收峰十分相似，但在～608cm－1处出现较大差别，以Sr2+、Ca2+和Ba2+部分A位取代La3+的钙铁矿型氧化物和B位Fe取代Mn时，由于离子的溶解能不同，对晶格的有序排列的影响程度不一，导致了Mn－O键的键力场不同，引起了吸收峰向低波数移动。这种结构上的差异，导致对汽车尾气中的有害成份碳氢化合物（HC）和一氧化碳（CO）的催化氧化能力降低。借此可以用于研究结构与催化性能的关系。     

原料杂质对堇青石窑具晶相结构与性能的影响

对重青石窑具原料中的CaO，TiO2，Fe2O3以及R2O（Na2O＋K2O）对窑具多晶结构与性能的影响进行研究，从而确定原料中的Cao，TiO2，Fe2O3和R2O允许的存在量为CaO（2．2～2．7）％，TiO2（1．0～1．5）％，Fe2O3（0．8）％和R2O≤0．9％。     

利用手持技术改进测定乙醇分子结构实验

利用压强传感器代替排水集气法,改进测定乙醇分子结构实验的仪器装置,并探索最佳反应条件。另外,设计两个空白实验,结合压强变化曲线对实验误差进行相关讨论。     

光谱仪测试范围的扩展

由于石化行业的生产需要，其材质的使用具有多样性和广泛性，经常会出现顾客委托的测试样品的一个或几个元素跨越光谱仪现有测试程序测量范围的情况。本法通过对光谱仪测试原理的认识，根据光谱仪的测试能力及标样的采集，实现了一个或几个元素测量范围的扩展，并对其测量的影响因素进行了研究。     

Influence of viscosity of medium on processes of oxygen quenching of excited states of mesoporphyrin

The oxygen quenching rate constants for singlet and triplet excited states of the dimethyl ester of mesoporphyrin IX increase with decreasing viscosity of the medium and reach a maximum at a viscosity of approximately 0.4 mPa·sec, after which the rate constants begin to decrease. The drop in rate constant with increasing fluidity of the medium may be related to a nonequilibrium character of the elementary act in the interaction of the reactants in the solvent cage. In viscous media such as isopropyl alcohol, isobutyl alcohol, and isoamyl alcohol, the reaction radius is greater than the sum of the radii of the reacting particles. The long-range character of these processes is due to the relatively weak dependence of the quenching probability on distance.Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 25, No. 2, pp. 161–167, March–April, 1989.     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

Neutral diterpenoids of oleoresins of five species of conifers of Transcarpathia

The compositions of the neutral diterpenoids of the oleoresins of five species of conifers growing in the Transcarpathia have been studied. It has been found that the oleoresins ofAbies alba M.,Larix decidua M., andPicea excelsa L. contain more than 50% of neutral diterpenoids. The group and qualitative compositions of the oxygen-containing diterpenoids have been determined. In the oleoresins ofAbies alba,Picea excelsa, andPicea abies tertiary alcohols — cis-abienol and isocembrol — predominate, while inLarix decidua the main component is the hydroxy ester larixyl acetate. Primary alcohols related to the resin acids have been found in all the oleoresins investigated. Features of the distribution of diterpenoids according to the species of conifers have been revealed. The results obtained are necessary for the chemotaxonomy of conifers of the family Pinceae.Novosibirsk Institute of Organic Chemistry, Siberian Branch, Academy of Sciences of the USSR. Translated from Khimiya Prirodynkh Soedinenii, No. 6, pp. 812–816, November–December, 1988.     

Determination of heats of detonation and influence of components of composite explosives on heats of detonation of high explosives

The heats of detonation of 20 simple high explosives and explosive mixtures were determined by means of an adiabatic detonation calorimeter designed by the authors. The results indicated that the performance of the instrument was reliable and the experimental data were very accurate. For explosive mixtures, there was a linear accumulative relationship between the heats of detonation of the explosive mixture and its components. Accordingly, the heats of detonation of explosive mixtures could be calculated directly from the heats of detonation of simple explosives and the characteristic heats of other components. The experiments showed that the gold or brass shell of the cylindrical charge could be substituted by a thick-walled porcelain shell, which had the advantage of cheapness.

     

物质分配系数的测定实验改进

实验教学目的是从解决实际问题出发,以实验技术训练和实验设计思想培养为目标。介绍了将单一的物质分配系数测定实验改进为综合实验,提高了实验效果及实验资源利用率。     

Calculation of enthalpies of hydrogenation of hydrocarbons

Sets of hydrogen molecule equivalents have been developed which permit the calculation of hydrogenation of different types of carbon-carbon bonds from ab initio total energies (3-21G and 6-31G* basis sets, and, to a more limited extent, for MP2/6-31G* data) of reactants and products. The calculated enthalpies of hydrogenation are in good agreement with experiment for unstrained molecules, with average errors on the order of 2 kcal/mol. The 6-31G* equivalents allow the enthalpies for strained molecules to be calculated accurately, but the 3-21G equivalents do not. The equivalents for both basis sets have been tested by calculating the enthalpies of hydrogenation of carbon-carbon bonds in nitrogen- and oxygen-containing organic molecules, free radicals, and classical carbocations. The results are in good agreement with experiment in most cases.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。