取代二茂铁多碘化合物的合成`表征和穆斯堡尔谱研究

合成了一系列新的取代二茂铁多碘化合物,通式为[(RC_5H_4)(R′C_5H_4)Fe]·I_x。元素分析表明,取代基不同时,二茂铁与碘可以整比或非整比结合。~(57)Fe穆斯堡尔谱和红外光谱的研究表明,因取代基不同,二茂铁可以完全地或部分地被碘氧化。     

二茂铁衍生物的合成、表征及猝灭Ru(bpy)_3~(2+)发光的研究

本文以邻菲罗啉和二茂铁为原料,合成了一系列新Schiff碱型二茂铁衍生物:(C_(10)H_6N_2)C=N—N=CR—Fe,(C_(10)H_6N_2)C=N—C_6H_4—N=CR—Fe,(C_(10)H_6N_2)C=N—C_6H_4—C_6H_4—N=CR—Fe,(R=H,CH_3,Fe为二茂铁基);并对其进行了元素分析和光谱表征.该类二茂铁衍生物能有效地猝灭Ru(bPY)_3~(2+)的发光,Stern-Volmer图呈线性关系,双分子猝灭过程速率常数k_q为10(?)dm~3/mol·s~(-1)数量级.猝灭过程按电子转移还原机理进行.     

一些含半夹心结构ⅥB族金属的1,1’-二硫(硒)二茂铁化合物的合成

CpCr(NO)(CO)_2与Fe(C_5H_4S)_2S反应,形成氧化-还原产物CpCr(NO)(SC_5H_4)_2Fe(1)。双杂核二茂铁化合物CpM(NO)(EC_5H_4)_2Fe[M=Mo,E=S(2a),Se(2b);M=W,E=S(4a),Se(4b)]、CpMo(NO)(SC_5H_4)_2Fe(3)、Cp_2Mo(SeC_5H_4)_2Fe(6)和Cp_2W(SC_5H_4)_2Fe(7)可通过Fe(C_5H_4ELi)_2·2THF(E=S,Se)与CpM(NO)I_2(M=Mo,W)、[CpMo(NO)I_2]_2或Cp_2MCl_2(M=Mo,W)反应制得。三核杂原子二茂铁化合物[CpCr(NO)_2]_2(EC_5H_4)_2Fe[E=S(8a),Se(8b)],由Fe(C_5H_4ELi)_2·2THF(E=S,Se)与二倍摩尔量的CpCr(NO)_2I反应制备。通过AgBF_4氧化2a得到二茂铁离子型化合物[CpMo(NO)(SC_5H_4)_2Fe]~ BF_4~-(5)。采用元素分析、红外光谱、~1H和~(13)C NMR谱以及EI-MS表征了所合成的新型化合物。     

环戊二烯基(或茚基)二氯化钕体系催化丁二烯聚合反应动力学

<正> 环戊二烯基(或茚基)轻烯土二氯化物C_5H_5NdCl_2·nC_4H_8O(C_5H_5为环戊二烯基、C_4H_8O为四氢呋喃、Ln代表Pr或Nd、n=0,1,2,3)、C_5H_5LnCl_2·HCl·nC_4H_8O、C_9H_7LnCl_2·nC_4H_8O和C_9H_7LnCl_2·HCl·nC_4H_8O(C_9H_7为茚基)能与烷基铝组合形成一类新型丁二烯聚合催化剂,虽然稀土催化丁二烯聚合反应动力学已有报道,但是其催化体系、聚合条件和研究方法各不相同。过去的研究多应用稳态动力学处理方法侧重于聚合速度的研究。本文的目的在于通过聚合物活性链的变化,考察C_5H_5NdCl_2·nC_4H_8O     

苯基稀土氯化物的合成及其表征

1970年,Hart等首先合成了Sc(C_6H_5)_3、Y(C_6H_5)_3、LiLa(C_6H_5)_4和LiPr(C_6H_5)_4。1972年,Cotton等测定了[Lu(2,6-(CH_3)_2C_6H_3)_4]·[Li·4THF]的晶体结构。1986年,陈文启等人合成了Nd(C_6H_5)_3,Gd(C_6H_5)_3和LiNd(C_6H_5)_4。本文首次合成了苯基稀土氯化物C_6H_5LnCl_2·nTHF(Ln=Pr,Sm,Gd,n=3,4);C_6H_5LnCl_2·LiCl·nTHF(Ln=Pr、Nd、Sm、Gd,n=2、3、5);(C_6H_5)_2GdCl·LiCl·2THF;[(C_6H_5)_2NdCl]_2·LiCl·4THF。测定了C_6H_5GdCl_2·4THF的晶体结构。     

二种国产C_(18)化学键合微粒HPLC固定相的性能

对天津化学试剂二厂生产的YWG—C_(13)H_(37)·5μ,YWG—C_(13)H_(37)·10±2μ,YWG—C_(13)H_(37)·10±1μ,用扫描电镜观察和对其色谱性能测试,与西德E.Merck公司生产的Lichrosorb—RP·18.5μ     

腙类配位化合物的研究——Ⅰ.乙酰基一和1,1′—二乙酰基二茂铁苯甲酰腙及其过渡金属螯合物的制备和性质

制备了两个二茂铁基芳酰基腙:乙酰基二茂铁苯甲酰腙,FcCMe=NNHCOC_6H_5(HL~Ⅰ)和1,1′--二乙酰基二茂铁苯甲酰腙,Fe(C_5H_4CMe=NNHCOC_6H_5)_2(H_2L~Ⅱ)。HL~Ⅰ和H_2L~Ⅱ与过渡金屑醋酸盐反应,得到两种螯合物:ML_2~Ⅰ和ML~Ⅱ[M=Co(Ⅱ)、Zn(Ⅱ)和Cd(Ⅱ)]。对这些螯合物的元素分析,差热热重分析、IR、UV及~1HNMR谱进行了详细讨论。     

废水中微量肼的测定

迭氮化钠生产排放的废水中含有大量亚硝酸乙脂(C_2H_5ONO)、迭氮化钠(NaN_3),和水合肼(N_2H_4·H_2O)等毒物。本法根据文献,基于N_2H_4与对二甲氨基苯甲醛作用,生成对二甲氨基苄连氮,在     

粉状白钨酸研究 Ⅸ.含W-N键的钨同多酸盐[Py_2W_(12)O_(38)]~(-4)的合成

继不久前McCarronⅢ自MoO_3·2H_2O和吡啶制得了[(C_5H_5N)_2MO_ 8O_(26)]~(4-)之后,我们通过粉状白钨酸与吡啶水溶液反应成功地制备了一种无色的晶体(C_5H_5NH)_4[(C_5H_5N)_2W_(12)O_(38)]·6H_2O。从反应混合物中还分离到一个黄色的副产物,其组成经分析为(C_5H_5N)_(0.85)·WO_3。与Johnson用黄钨酸制备的层状化合物(C_5H_5N)·WO_3属同一物相。粉状白钨酸在无水吡啶中放置两周后可得到另一种化学式为(C_5H_5NH)HW_4O_(13)·3H_2O的吡啶化合物,经IR和DTA研究可初步说明该化合物与粉状白钨酸(微晶态)之间的联系,并因此推测白钨酸的组成可能为H_2W_4O_(13)·nH_2O。     

1,1′-二硒取代二茂铁衍生物的合成

由1,2,3-三硒[3]桥二茂铁(Ferrocenophane)经LiAlH_4还原生成二硒酚,不经分离直接与一亲电试剂在三乙胺存在下反应,得到7种1,1′-二硒醚二茂铁,4种1,n-二硒[n]桥二茂铁(n=3～5)和1种螺形化合物[Fe(C_5H_4Se)_2]_2Sn。这12种化合物中有7种尚未见文献报道,对其中几种产物进行了~(77)Se NMR谱及质谱分析。讨论了影响产率的因素和核磁共振图谱。     

HEPT类化合物的QSAR研究

为定量结构／活性相关性研究提取了量子化学参数,拓扑指数Am,分子连接性指数^mxt及疏水性常数,同时应用正交变换和最佳变量子集算法（Leaps-and-Bonds)进行了变量压缩和选择,进而实施了多元回归分析,并由此结果进行了HEPT类化合物（1－[(2-hydroxyethoxy)methyl]-6-(phenylthio)-thymine derivatives)的结构／活性关系的理论解释,进行了人工神经网络法对于该类化合物的活性预测,其结构明显好于多元回归法。     

From the Micro- to the Macro-: Managing the Conservation of the Warship,Vasa

Sweden's famous warship, Vasa, sank on her maiden voyage in August 1628, and remained on the bottom of Stockholm harbour for 333 years. Raised in 1961, she became the first large-scale wooden object to be treated with polyethylene glycol (PEG). In the summer of 2000 a number of acidic salt precipitations were noticed on the surface of the ship and on wooden artefacts in the storerooms. An international research project has been established to look into the causes of this problem and suggest possible re-treatments. Meanwhile projects are underway to monitor movements in the ship, to build a better support system, and to replace the thousands of iron bolts holding the structure together, while a sophisticated new climate system has recently been installed in the museum.     

液滴荧光传感与计算机联用技术在微量分析中的应用

通过在LS55型荧光-磷光-发光分光光度计上加装液滴产生及调节附件,采用计算机采集与分析处理数据,成功地研制了双通道液滴光化学传感装置.利用葡聚糖凝胶对复合维生素B中不同组分的选择性吸附来达到分离与同时检测的目的,并将其用于复合维生素B药片的分析,取得了满意的结果.     

On the scaling of the interface energy of the liquid clusters in the disordered nanoporous medium

Similarity of the extrusion curves of non-wetting liquid in a nanoporous medium with different initial fill volume fractions is observed experimentally. The similarity can be explained by the scaling of the interface energy and the self-similarity of the infinite percolation cluster of fluid-filled pores. Understanding the physical processes leading to the observed phenomena is a foundation for the development of high-performance devices for damping and energy storage on the basis of such heterogeneous systems.     

光亮剂对银电沉积行为的影响

用电势阶跃法和旋转圆盘电极法 (RDE)以及SEM和XRD测试手段 ,初步研究了光亮剂对氰化体系中银电沉积行为的影响 .研究表明 ,光亮剂的加入并未导致银电沉积成核机理的改变 ,但显著增强了镀液的微观平整效应 ,并且所得镀层的表观光滑程度明显改善 .XRD测试亦同时表明光亮剂的加入并未改变镀层的择优取向     

Using of the Agglomeration-in-liquid for the Technology of the Fine Materials

The content of the fine and ultrafine particles in the raw material results in difficulty of the separation, the loss of the valuable components and ecological contamination. Secondary using of the fine particles is impossible without their granulation. This problem has been solved by the agglomeration-in-liquid method.An agglomeration-in-liquid method is a process to produce agglomerates in a liquid phase from solid particles suspended in the liquid. The surface of solid particles and the binding liquid must be of identical polarity, but the continuous phase must be of the opposite polarity. The water solutions of the surfactant are the binding liquids or the organic liquids.     

Influence of the Position of the Connecting Spacer of the Chromophore on the Nonlinear Optical Response

A new chromophore, C1 , based on a similar DπA‐structure as in the FTC ‐chromophore but with a hydroxyalkyl spacer perpendicular to the direction of the dipole moment was synthesized. Both chromophores and the CLD ‐chromophore were used to prepare high T_g nonlinear optical vinyl polymers. The influence of the position of the spacer on the DπA‐system on the NLO response of the resulting polymers was investigated.

     

On the dependence of the critical supersaturation on the initial undersaturation in the reverse Wilson chamber

The dependence of the critical supersaturation on the degree of the initial undersaturation has been analyzed in detail.This dependence is explained by means of the Richarch-Powell equation, taking into account the dependence of the -ratio upon the partial pressures of the inert gas and the liquid under investigation.     

Copper-containing dendromesogens: the influence of the metal on the mesomorphism

The synthesis and liquid crystalline behaviour of the first and second generations of a dendrimeric structure based on poly(propyleneimine)(DAB-dendr(NH₂)_x) are reported. 4-(4-n-Alkoxybenzoyloxy)salicylaldehydes are used as mesogenic moieties attached at the peripheral amino groups of the dendrimers giving rise to dendromesogens with four and eight mesogenic branches. From these dendromesogens, considered as organic ligands, were prepared six metal-containing dendrimers which incorporate two or four copper atoms in their structures. All the dendrimeric ligands and three of the metal-containing dendrimers exhibit liquid crystalline properties which were studied by optical microscopy, DSC, X-ray diffraction and EPR spectroscopy.