反相离子对高效液相色谱法测定母粉及母液中的杀鼠新

用反相离子对高效液相色谱法测定了杀鼠新母粉及母液中有效成份含量。采用Partisil-10ODS色谱柱，以甲醇：离子对溶液＝80：20（体积比）为流动相，离子对溶液为0.005mol/L四丁基铵磷酸盐（pH为7.5)的缓冲溶液，测定波长285nm。方法在0.025-0.15g/L范围内有很好的线性关系。杀鼠新母粉和母液的相对标准偏差分别为1.24%、0.77%(n=7)，回收率分别为：母粉,97.7%-99.8%；母液，98.5%-100.4%。     

胺型键合反相固定相的制备及评价

首次将一种新型硅烷偶联剂--β-（3，4-环氧环已基）乙基三甲氧基硅烷（β-ECTS）与辛胺反应，然后再键合到硅胶上，得到了胺型键合固定相，并用元素分析、^13C固体核磁共振、红外光谱进行了表征。以甲醇和水为二元流动相，用包括碱性、酸性和中性有机化合物在内的混合物对该固定相进行评价，并考察了该填料的适用pH范围及水解稳定性。结果表明，该固定相具有较好的色谱性能，且在pH=2-8之间稳定性能良好，可有效地用于碱性化合物的分析分离。     

New Type High Efficient Quasi-Solid-State Ionic Liquid Electrolyte for Dye-Sensitized Solar Cells

For the fist time the preparation of a mostly solid-state high efficiem electro-conductive material comprising 1-methyl-3-propylimidazolium iodide （MPII）, benzimidazole （BI）, iodine and lithium iodide was reported. In this electrolyte, BI acts as not only additives but also gelators. With its significant electrochemical properties, an overall efficiency of 3.07% was achieved under AM 1.5 （100 mW/cm^2）.     

硝基甲烷在离子液体BMImBF4中的电还原特性

采用循环伏安等测试方法, 以铂微盘电极为工作电极, 研究了硝基甲烷在离子液体1-正丁基-3-甲基咪唑四氟硼酸盐(BMImBF4)中的电化学行为, 并探讨了温度和扫描速率等因素对硝基甲烷电化学特性的影响. 实验结果表明, 硝基甲烷在离子液体BMImBF4中的还原反应是受扩散控制的不可逆过程. 估算了不同温度下硝基甲烷在离子液体BMImBF4中的扩散系数D, 进而求得它的扩散活化能Ea约为39.5 kJ·mol-1.     

农药甲霜灵对映体的高效液相色谱分离及手性拆分热力学研究

以正己烷 异丙醇为流动相 ,在纤维素 三 (3 ,5 二甲基苯基氨基甲酸酯 ) (CDMPC)涂敷型手性固定相上 ,对农药甲霜灵外消旋体进行了拆分 ,考察了流动相组成、柱温等对甲霜灵对映体的保留和分离的影响 ;对甲霜灵R、S对映体与固定相之间的保留和分离的热力学机理进行了讨论     

低压离子色谱法测定土壤中速效钾

通常对土壤中速效钾的测定方法所用仪器昂贵。而低压离子色谱分析仪结构简单,操作简便,速度快,灵敏度高,价格低[1]。本文通过试验,确立了低压离子色谱法测定土壤速效钾的最佳条件,对实际样品的测定结果与推荐值呈显著相关性。1　实验部分土壤经风干、研磨,过100目土壤筛,测定其水份系数[2],贮存于密闭玻璃瓶内备用。准确称取2 0000g土样于50ml烧杯内,加20ml提取剂(0 05mol/LHCl+0 0125mol/LH2SO4),摇匀,25℃提取25分钟,离心分离。连接色谱仪、记录仪、蠕动泵(图1)。自制2J 3低压离子色谱仪,量程10×10μs,蠕动泵流速10刻度,记录仪量…     

二苯并18－冠－6辅助钡离子在1，2－二氯乙烷／水微界面转移的伏安研究

应用液／液界面微电极对二苯并１８－冠－６（ＤＢ１８－Ｃ－６）辅助推动Ｂａ~（２＋）在１，２－二氯乙烷／水（ＤＣＥ／Ｗ）界面转移的电化学过程进行了详细探讨，证明该过程遵循ＴＩＣ机理，是受扩散控制的可逆过程。通过转移电流和反应物浓度之间的线性关系，测定了Ｂａ~（２＋）以及用其它方法难以测定的ＤＢ１８－Ｃ－６。     

使用手性冠醚及手性柱的HPCE和HPLC法拆分伯胺类药物对映体的对比研究

报道了在缓冲液中添加 1 8-冠 - 6 -四甲酸 (1 8C6 H4 )的高效毛细管电泳法(HPCE)对 8个含氨基的药物进行拆分 ,低 p H值 (2 .0 6 )和较高浓度的 Tris缓冲液(2 0 mmol· L- 1)可加快手性分离。用手性柱 Crownpak CR(+)的高效液相色谱(HPLC)法对与前相同的 8个含氨基药物进行拆分 ,甲醇浓度增大 ,分离度 RS值有所减小。实验结果还表明 ,使用 HPCE法拆分的各物质 RS值大于使用 HPLC法拆分相应物质的 RS值。     

SAXS investigations on chiral liquid crystalline polymers: antiferroelectric and ferrielectric structures?

The structure and phase behavior of liquid crystalline polymers (LCPs) having a common chiral side chain mesogen but different main chain structures have been investigated using small-angle X-ray scattering (SAXS). While the low molecular weight chiral side chain mesogen by itself exhibits ferroelectricity, the SAXS data of the side chain LCP with a flexible polyacrylate backbone contains a bilayered superstructure peak that is indicative of antiferroelectric order. The combined LCP with a nonpolar main chain mesogen also has a bilayered superstructure, but has a different structural organization in the proposed antiferroelectric phase compared to the side chain LCP. Further changes in the phase behavior and structural organization occur when a polar group is introduced into the main chain mesogen. A ferrielectric phase has been proposed to explain the observation of a trilayered superstructure in the corresponding SAXS data. The influence of the chemical structure and connectivity on the phase behavior and superstructure formation in the chiral LCPs is discussed.     

Analytical characteristics of combined gas chromatographic systems: Packed precolumn-open tubular column

The peculiarities of the flow splitting technique for sample injection into a capillary column have been discussed. A comparative investigation of reproducibility of the analytical results obtained for two gas chromatographic systems using flow splitting [1) sample injector-packed predolumn-splitter-open tubular capillary column and (2) sample injector-splitter-open tubular capillary column] has been carried out. It was experimentally shown that the first system ensures considerably better reproducibility for the results concerning the composition of the analyzed mixtures. Other advantages of the first system are also discussed.