Trace enrichment and HPLC analysis of polycyclic aromatic hydrocarbons in environmental samples,using solid phase extraction in connection with UV/VIS diode-array and fluorescence detection

Summary Both the separation of polycyclic aromatic hydrocarbons (PAH's) on tailor made HPLC phases, and their chromatographic enrichment and quantitative determination are of great interest. Because of the generally low concentrations of PAH's in the environment, and the low limiting values in German legislation for drinking water, methods for selective enrichment and sensitive detection are indispensable. On account of their relatively high amounts in soil, the determination of PAH's is valuable for the assessment of the potential danger to ground water by waste materials. These requirements can be fulfilled by used of solid phase extraction on enrichment columns, and fluorescence or UV/VIS diode array detection. For the detection of PAH's in the picogram range, the wavelengths for excitation and emission were time programmed over the chromatogram. With this feature, it is possible to detect all the individual compounds at the highest sensitivity, over the entire analysis.     

手性配体立体选择性萃取分离扁桃酸对映体

Based on chiral ligand exchange, the distribution behavior of mandelic acid enantiomers in the two-phase system containing copper ion(Ⅱ)(Cu²⁺) and N-n-dedecane-L-hydroxyproline (L), was studied. At different pH, the partition of Cu²⁺ in the two-phase system containing N-n-dedecane-L-hydroxyproline, was investigated. The formation constant of binary cpmplex(Li₂Cu) was obtained by regression. The influence of pH, concentrations of Cu²⁺ and chiral ligand, and solvents on partition coefficients(K) and separation factor(α), was discussed. The experimental results show that Li forms more stable ternary complex with D-mandelic acid than with L- mandelic acid. There is a large influence of pH on K and α. At low pH values (<3.5), formation of binary complexes is thermodynamically unfavourable. K and α are best when pH values are above 3.5 and the molar ratio of chiral ligand to Cu²⁺ is 2∶1. At the same time, solvents influence K and α very much.     

Cyanex 923-H2SO4体系萃取第3相的形成和应用

三相体系;Cyanex 923-H2SO4体系萃取第3相的形成和应用     

LiCoO2中锂离子固相扩散系数随循环次数的变化

The solid diffusion coefficient of lithium-ion in LiCoO₂ cathode material has been investigated by the capacity intermittent titration technique (CITT) at different voltages and at different charge/discharge cycles. By SEM, XRD and FTIR techniques, the structure of LiCoO₂ was studied before and after charge-discharge cycles, and the relationship between solid diffusion coefficient and crystal structure was further discussed. CITT results show that the value of Li⁺ solid diffusion coefficient of LiCoO₂ is about 10^-12 cm²·s^-1. During the whole charge-discharge cycles, the Li⁺ solid diffusion coefficient decreased within the voltage of 4.0～4.3 V, which is attributed to the change of the structure of LiCoO₂.     

微波辐射下蒙脱土K10固载氯化铁氧化二芳基乙醇酮

微波辐射下以蒙脱土K-10固载氯化铁为氧化剂, 氧化二芳基乙醇酮生成二芳基乙二酮化合物, 反应时间短, 产率高, 操作简便, 污染小, 是一种有效的由二芳基乙醇酮氧化制备二芳基乙二酮的方法.     

WS2 超细粉体的固相法合成

WS2 超细粉体的固相法合成;WS2;固相反应;过硫系数;高能球磨;粒度     

铁－铜－锰氧化物／海泡石催化剂对苯羟基化为苯酚的催化作用

铁－铜－锰氧化物／海泡石催化剂对苯羟基化为苯酚的催化作用曹声春，黄孟光，李克，杜兴军（湖南大学化工系，长沙４１００８２）关键词氧化铁，氧化钢，二氧化锰，海泡石，负载型催化剂，苯，羟基化，苯酚由苯合成苯酚的现行方法存在着反应步骤多，工艺过程复杂，总转化...     

Chiralcel OD-RH手性柱拆分卡维地洛对映体

采用Ch iralcelOD-RH(纤维素3,5-二甲基苯基氨基甲酸酯)手性固定相高效液相色谱法研究了乙腈-高氯酸钠缓冲盐体系对卡维地洛的手性拆分情况,讨论了流动相的各个因素(有机相的种类和比例、缓冲盐浓度、酸度等)对手性拆分的影响。在乙腈-高氯酸钠缓冲盐(pH 5.5,50 mmol/L)的体积比为35∶65的色谱条件下,卡维地洛对映体获得了基线分离。     

金属富勒烯La＠C_（2n）的合成、提取及其ESR和MS表征

采用对掺入Ｌａ_２Ｏ_３的石墨棒原位活化并结合交换电极回放方法制备了产率较高的金属富勒烯，并用甲苯高温热提取的方法有效地提取出Ｌａ＠Ｃ_（２ｎ），其中Ｌａ＠Ｃ_（７４）为可溶性金属富勒烯增加了新成员．同时，首次采用解吸电子轰击质谱对提取物进行了表征，讨论了提取物的ＥＳＲ谱．