室温下快速合成超小Fe3+掺杂BiF3纳米粒子

室温下快速合成了Fe³⁺掺杂的BiF₃超小纳米粒子,只需要反应1 min,较小的Fe³⁺离子即可替代BiF₃晶格中较大的Bi³⁺离子.随着Fe³⁺掺杂量的增加,BiF₃：Fe³⁺纳米粒子的粒径不断减小,当Fe³⁺的掺杂量达到0.119时,可以得到尺寸约为6.9 nm的Fe³⁺掺杂BiF₃超小纳米粒子.此外,Fe³⁺离子的掺杂使BiF₃：Fe³⁺-x样品的能带结构发生了显著变化.制备的Fe³⁺掺杂BiF₃超小纳米粒子在光催化剂和荧光材料方面具有潜在的应用价值.     

室温离子液体在聚合反应中的应用

室温离子液体作为一种环境友好的“绿色溶剂”,具有很多独特的物理化学性能,可以应用于自由基聚合、阳离子聚合、配位聚合、电化学聚合等反应体系。本文介绍了室温离子液体在上述反应中的应用。     

补骨脂素、异补骨脂素的固体表面室温燐光分析法

建立了以滤纸为基质的中草药有效成分补骨脂素、异补骨脂素的固体表面室温燐光 分析法。对影响室温燐光强度的各种因素进行了详细的研究，实验表明，补骨脂素的线性范围 为２×１０－６～２×１０－４ｍｏｌ／Ｌ；检出限为０．４７ｎｇ／斑，异补骨脂素的线性范围为４×１０－６～４×１０－４ｍｏｌ／Ｌ；检出限为０．１７ｎｇ／斑。     

12种嘌呤类化合物的滤纸基质室温燐光法研究

较为详细地研究了１２种嘌呤类化合物以滤纸为基质的室温燐光（ＲＴＰ）光谱特性与分子结构的关系，以及重原子效应和酸度效应对ＲＴＰ的影响。     

6-磺酰氯香豆素的室温燐光特性

通过多种重原子微扰剂和实验条件的选择,成功地实现了C6SCl在数种基质上的RTP发射。发现Pb(Ⅱ)盐是这种RTP发射的最有效的外部重原子微扰剂。在滤纸基质上,以1mol/L Pb(Ac)_2作重原子微扰剂获得了强度高且信/背比亦高的RTP信号,λ_(ex)/λ_(em)=320/496nm。0.2μl点样体积中,C6SCl含量在4～200pmol范围内与RTP信号强度呈良好的线性关系。     

Crystal Structures and Selected Properties of CoII Containing Thiostannates prepared by a New Room Temperature Route

The room temperature reaction of Na₄Sn₂S₆ · 5H₂O with CoCl₂ · 6H₂O and 2-(aminomethyl)pyridine (2-AMP) or trans-1,2-diamino-cyclohexane (DACH) leads to crystallization of two compounds with the compositions [Co(2-(aminomethyl)pyridine)₃]₂ Sn₂S₆ · 10H₂O ( 1 ) and [Co(trans-1,2-diaminocyclohexane)₃]₂Sn₂S₆ · 8H₂O ( 2 ). In both compounds [Sn₂S₆]^4– anions are present that are charge balanced each by two Co²⁺ centered complexes. Each of the two Co^II cations are sixfold coordinated by six N atoms of three 2-AMP or DACH ligands within slightly distorted octahedra. In compound 1 , the two complexes are linked by one [Sn₂S₆]^4– anion via strong N–H ··· S hydrogen bonds into centrosymmetric charge neutral trimeric units, that are further linked by weak C–H ··· S and N–H ··· S hydrogen bonds into chains that are directed along the a axis. These chains are further joined by N–H ··· O and O–H ··· O hydrogen bonds into a 3D network, with the H₂O molecules forming chains along the b axis. The crystal structure of 2 is similar to that of 1 featuring trimeric units which are also linked into chains. Between the chains water molecules are embedded that link the chains into a 3D network. Upon heating 2 in a thermobalance the water and ligand molecules are removed in discrete steps, indicating that compounds with more condensed thiostannate networks will form.     

离子液体反应介质中3-羟基丙酸甲酯加氢反应研究

以室温离子液体[Bmim]PF6作为反应介质,研究了四羰基钴钾K[Co(CO)4]催化3-羟基丙酸甲酯(3-HPM)加氢制1,3-丙二醇(1,3-PDO)的反应,并对反应条件进行了优化.同有机溶剂作为反应介质相比,该体系具有更高的选择性和更好的催化活性,并且产物经水萃取便可实现催化体系的回收利用.在反应温度165℃、氢气压力10.5 MPa、反应时间10 h、咪唑为促进剂的较佳反应条件下,3-HPM的转化率可达99.4%,1,3-PDO的收率可达82.9%,催化剂重复使用3次,1,3-PDO的收率不低于70%.并根据实验结果,提出了可能的催化反应机理.     

芦丁、丹皮酚固体表面延迟荧光分析法

建立了以滤纸为基质的中草药有效成分芦丁、丹皮酚的固体表面延迟荧光分析法（roomtemperaturedelayedfluorimetry,RTDF）。对影响延迟荧光强度的各种因素进行了详细的研究,实验表明,芦丁的线性范围为5×10~(－6)~1×10~(-4)mol/L,检出限为0．52ng／斑,丹皮酚的线性范围为1×10~(－6)~1×10~(-3)mol/L,检出限为0．08ng/斑。     

Room Temperature Synthesis of New Thiostannates by Slow Interdiffusion of Different Solvents

The new compounds [Ni(L₁)][Ni(L₁)Sn₂S₆]_n · 2H₂O ( I ) and [Ni(L₂)]₂[Sn₂S₆] · 4H₂O ( II ) containing the macrocyclic ligands L₁ (L₁ = 1,8-dimethyl-1,3,6,8,10,13-hexaazacyclotetradecane) and L₂ (L₂ = 1,8-diethyl-1,3,6,8,10,13-hexaazacyclotetradecane) were prepared at room temperature by overlaying an aqueous solution of Na₄SnS₄ · 14H₂O with the [Ni(L₁)](ClO₄)₂ complex dissolved in CH₃CN ( I ) or by overlaying a solution of the [Ni(L₂)](ClO₄)₂ complex dissolved in DMSO with an aqueous solution of Na₄SnS₄ · 14H₂O ( II ). The slow interdiffusion of the two solvents guarantees supersaturation in the interface region of the solvents so that crystallization of the compounds occurs. In the structure of I one Ni²⁺ cation has bonds to S^2– anions of the thiostannate anion thus generating chains along [100]. This cation is in an octahedral environment of four N atoms of L₁ and two S atoms of the [Sn₂S₆]^4– anion. The second [Ni(L₁)]²⁺ complex exhibits a square-planar coordination geometry. These [Ni(L₁)]²⁺ complexes and water molecules are located between the chains. In the structure of II isolated [Sn₂S₆]^4– anions and [Ni(L₂)]²⁺ cations are observed. The Ni²⁺ cations are fourfold coordinated by N atoms of the L₂ ligand and feature also a square planar environment.     

可可碱、咖啡因、茶碱的滤纸基质室温燐光测定

以快速定量滤纸为基质 ,用KI NaAc为重原子微扰剂 ,建立了测定痕量可可碱、咖啡因、茶碱的滤纸基质室温磷光 (PS RTP)分析法。该法取样量少 ,线性范围宽 ,可可碱、咖啡因、茶碱的线性范围分别为 14 4～5 76 ;5 .4 4～ 6 99;7.2 1～ 36 0ng/斑点 ;检出限分别为 1 14、0 78、1 80ng/斑点。该方法用于巧克力中可可碱、茶叶中咖啡因、氨茶碱药片中茶碱的测定 ,操作简便快速 ,选择性好。标准回收率在 92 8%～ 10 6 %之间 ;相对标准偏差RSD <5 %     

碳纳米管在室温熔盐中的电容特性

研究了碳纳米管在室温熔盐二(三氟甲基磺酸酰)亚胺锂(LiTFSI)-乙酰胺中的电容特性. 将碳纳米管制成薄膜电极, 以LiTFSI-乙酰胺为电解液, 装配成模拟电容器, 用循环伏安和恒流充放电法研究其电化学性能. 结果表明, 碳纳米管在室温熔盐中表现出典型的电容特性, 其比电容为22 F•g^-1, 模拟电容器的工作电压可达2.0 V, 具有非常好的循环性能, 循环充放电1000次后容量损失仅10%, 表明室温熔盐是超级电容器非常有前景的新型电解液.     

Synthesis and Modulated Crystal Structure of KBaNbS4

Single crystals of KBaNbS₄ have been prepared by the reaction of Nb with an in situ formed melt of K₂S₃, BaS, and S at 500 °C. Satellite reflections observed in X‐ray diffraction experiments of these crystals indicate the presence of a one‐dimensional lattice distortion. The modulated structure has been solved and refined from X‐ray data using the superspace group approach. KBaNbS₄ can be described in the (3 + 1)‐dimensional superspace group Pnma(α00)0s0 with lattice parameters a = 9.187(1), b = 7.001(1), and c = 12.494(1) Å and a modulation vector q = (0, 0.629(1), 0). In the structure the NbS₄ tetrahedra are stacked along the a axis and show a slight tilting against each other. The K⁺ and Ba²⁺ ions follow this tilting, both are slightly shifted from their positions in the average structure. The modulation does not lead to a significant change in the coordination spheres of the metal atoms. The small effects of the modulation correspond to the relatively weak intensities of the satellite reflections. Results of temperature dependent X‐ray investigations indicate that K⁺ librates at higher temperatures and the surrounding S^2? anions follow this motion. With decreasing temperature the libration of K⁺ is reduced and the coordination geometry freezes under formation of an incommensurate modulation. The heavier Ba and Nb atoms are also affected by positional modulation of the substructure and accommodate to their environment.     

用固体基质室温燐光法分析环境样品中多环芳烃的研究

用滤纸基质室温燐光法分析多环芳烃。以醋酸铊TlAc/醋酸铅Pb(Ac)_2(1∶1mol)的乙醇水(50％V/V)溶液为重原子微扰剂,对国产分析滤纸,玻璃纤维滤膜和醋酸纤维滤膜等9种不同的基质材料测定芘的燐光信号强度并进行了比较。对芘、荧蒽、苯并(e)芘、苯并(a)芘、苯并(ghi)芘和晕苯的混合物样品进行了测定。对煤飞灰和燃煤排放物样品中的芘和苯并(a)芘进行了定量分析,并用高效液相色谱法对测定结果进行验证。对芘和苯并(a)芘的检测限分别达到10~(-10)和10~(-9)g数量级。本文还对进一步提高灵敏度的问题进行了讨论。     

中草药有效成分山姜素的固体表面室温磷光法研究

本文选择滤纸作基质，以ＬｉＡｃ作重原子微扰剂，建立了测定中草药中痕量有效成分山姜素的滤纸表面室温磷光法。该法取样量少（２μＬ），线性范围宽（２．９～５８０ｎｇ／斑），灵敏度高（检出限０．４０ｎｇ／斑），操作简便、快速。     

4种喹诺酮类药物滤纸基质室温光法研究

提出了以滤纸为基质的环丙沙星、氟罗沙星、洛美沙星和氧氟沙星4种喹诺酮类药物的滤纸基质室温光(PS-RTP)分析的新方法. 方法取样量少(1.5 μL).其线性动力学范围依次为0.11～55.2、0.35～211、2.10～526 、1.03～411(ng/斑点);灵敏度高,其检出限分别为0.082、0.070、0.080、0.123(ng/ 斑点);标准回收率在97.70%～102.2%之间.相对标准偏差RSD＜1.8%.     

Application of Modulated Temperature DSC to Distillate Fuels and Lubricating Greases

In this work the usefulness of Modulated Temperature DSC (MTDSC) for characterizing petroleum products is illustrated with some typical examples of recent applications. Specifically, the reliability of the method is outlined on the basis of the freezing behaviour of distillate fuels and the thermal analytical characterization of lubricating greases. The results of experiments performed on the evaporation residue of distillate fuels, aimed at providing insights into the structure of degradation products, will also be presented. The experiments were carried out using a DSC 2910 module from TA Instruments Inc., upgraded with the MTDSC option. The samples were exposed to a cyclic heating profile which was generated by an underlying heating (or cooling) rate of 2°C min⁻¹ while superimposing a sinusoidally varying time-temperature wave with an amplitude of ±0.5°C and a period of 40 s. This revised version was published online in August 2006 with corrections to the Cover Date.     

离子液基萃取金属离子的研究进展

室温离子液体作为一种新型绿色溶剂,因其具有不挥发、不易燃等重要特性,故近年来在各种金属离子液/液萃取领域的应用日益受到关注。本文系统评述了离子液基萃取金属离子的分配规律、萃取机理、缺陷和克服方法,并展望了该分离方法在环境分析化学领域的应用前景。     

茶叶中咖啡因的纸基质室温燐光法体内药代动力学研究

以快速定量滤纸为基质 ,用KI NaAc为重原子微扰剂建立了测定痕量咖啡因的滤纸基质室温光(PS RTP)分析法。并用于茶叶中咖啡因的测定及其在人体内的药代动力学研究。实验表明 :PS RTP法用于茶叶中咖啡因的测定准确、灵敏。受试者饮茶后 1～ 2h尿样中咖啡因排泄达高峰 ,2 4h后基本排泄完毕。咖啡因的尿排泄量占总摄取量的 64 .2 5 %。     

室温磷光免疫分析研究的进展

对磷光免疫分析研究现状和发展趋势,作简要的概述,并对开展固体基体室温磷光免疫分析的可能性和优势,及其采用多发光分子微球作标记物的几种技术作了介绍,引用文献36篇。     

离子液体在萃取分离中的应用研究进展

室温离子液体作为一种新型绿色溶剂,具有液程宽、几乎不挥发、溶解能力强及结构可调等独特的物理化学性质,近年来逐渐被人们认识了解,它在各个领域的应用也得到了初步的发展.本文重点概述了离子液体在萃取分离金属离子方面的研究进展,并对离子液体萃取分离有机物和生物分子的研究作了简要介绍.引用文献54篇.