A method for rapid and simultaneous determination of imidazolium and pyridinium ionic liquid cations by ion-pair chromatography with ultraviolet detection was developed. Chromatographic separations were performed on a...A method for rapid and simultaneous determination of imidazolium and pyridinium ionic liquid cations by ion-pair chromatography with ultraviolet detection was developed. Chromatographic separations were performed on a reversed-phase silica-based monolithic column using 1-heptanesulfonic acid sodium-acetonitrile as mobile phase. The effects of ion-pair reagent and acetonitrile concentration on retention of the cations were investigated. The retention times of the cations accord with carbon number rule. The method has been successfully applied to the determination of four ionic liquids synthesized by organic chemistry laboratory.展开更多
研究了用硅胶整体柱和直接电导检测的离子对色谱快速分析高氯酸盐的方法。实验采用Chromolith Speed ROD RP-18e色谱柱，以氢氧化四丁铵（离子对试剂）＋邻苯二甲酸＋乙腈（有机改进剂）为淋洗液，讨论了离子对试剂浓度、有机改进剂浓度...研究了用硅胶整体柱和直接电导检测的离子对色谱快速分析高氯酸盐的方法。实验采用Chromolith Speed ROD RP-18e色谱柱，以氢氧化四丁铵（离子对试剂）＋邻苯二甲酸＋乙腈（有机改进剂）为淋洗液，讨论了离子对试剂浓度、有机改进剂浓度、pH、色谱柱温度和流速对ClO4^-保留时间的影响。确定最佳色谱条件为：0．25mmol／L氢氧化四丁铵＋0．18mmol／L邻苯二甲酸＋7％乙腈（pH5．5）作为淋洗液，柱温30℃，流速6．0mL／min。在此条件下，ClO4^-的保留时间在1min之内。其它常见阴离子（Cl^-、NO3^-、SO4^2-和I^-）不干扰测定。方法的检出限为1．56mg／L；工作曲线的线性范围是2．4～100mg／L；峰面积的相对标准偏差（RSD，n=5）为1．9％。将本方法应用于测定加标果汁和加标地下水中的ClO4^-，加标回收率分别为98．2％和97．6％。展开更多
A method was developed for the determination of tetraethyl ammonium （TEA） by reversed-phase ion- pair chromatography with indirect ultraviolet detection, Chromatographic separation was achieved on a reversed-phase C...A method was developed for the determination of tetraethyl ammonium （TEA） by reversed-phase ion- pair chromatography with indirect ultraviolet detection, Chromatographic separation was achieved on a reversed-phase C18 column using background ultraviolet absorbing reagent - ion-pair reagent - organic solvent as mobile phase. The effects of the background ultraviolet absorbing reagents, detection wavelength, ion-pair reagents, organic solvents and column temperature on the determination method were investigated and the retention rules discussed. Results found that TEA could be successfully analyzed by using 0.7 mmol/L 4-aminophenol hydrochloride and 0.15 mmol/L 1-heptanesulfonic acid sodium mixed with 20% （v/v） methanol as mobile phase at a UV detection wavelength of 230 nm. Under these conditions, the retention time of tetraethyl ammonium was 2.85 min. The detection limit （S/N = 3） for TEA was 0.06 mg/L. The relative standard deviations （n = 5） for peak area and retention time were 0.35% and 0.02%, respectively. The method has been successfully applied to the determination of synthesized tetraethyl ammonium bromide. Recovery of tetraethyl ammonium after spiking was 99.1%.展开更多
基金supported by the Natural Science Foundation of Heilongjiang Province(No.B200909)the Program for Scientific and Technological Innovation Team Construction in Universities of Heilongjiang Province(No. 2011TD010)
文摘A method for rapid and simultaneous determination of imidazolium and pyridinium ionic liquid cations by ion-pair chromatography with ultraviolet detection was developed. Chromatographic separations were performed on a reversed-phase silica-based monolithic column using 1-heptanesulfonic acid sodium-acetonitrile as mobile phase. The effects of ion-pair reagent and acetonitrile concentration on retention of the cations were investigated. The retention times of the cations accord with carbon number rule. The method has been successfully applied to the determination of four ionic liquids synthesized by organic chemistry laboratory.
文摘研究了用硅胶整体柱和直接电导检测的离子对色谱快速分析高氯酸盐的方法。实验采用Chromolith Speed ROD RP-18e色谱柱，以氢氧化四丁铵（离子对试剂）＋邻苯二甲酸＋乙腈（有机改进剂）为淋洗液，讨论了离子对试剂浓度、有机改进剂浓度、pH、色谱柱温度和流速对ClO4^-保留时间的影响。确定最佳色谱条件为：0．25mmol／L氢氧化四丁铵＋0．18mmol／L邻苯二甲酸＋7％乙腈（pH5．5）作为淋洗液，柱温30℃，流速6．0mL／min。在此条件下，ClO4^-的保留时间在1min之内。其它常见阴离子（Cl^-、NO3^-、SO4^2-和I^-）不干扰测定。方法的检出限为1．56mg／L；工作曲线的线性范围是2．4～100mg／L；峰面积的相对标准偏差（RSD，n=5）为1．9％。将本方法应用于测定加标果汁和加标地下水中的ClO4^-，加标回收率分别为98．2％和97．6％。
基金supported by the Natural Science Foundation of Heilongjiang Province(Grant No.B201307)the Ministry of Education of Heilongjiang Province(No.12531192)the Program for Scientific and Technological Innovation Team Construction in Universities of Heilongjiang Province(No. 2011TD010)
文摘A method was developed for the determination of tetraethyl ammonium （TEA） by reversed-phase ion- pair chromatography with indirect ultraviolet detection, Chromatographic separation was achieved on a reversed-phase C18 column using background ultraviolet absorbing reagent - ion-pair reagent - organic solvent as mobile phase. The effects of the background ultraviolet absorbing reagents, detection wavelength, ion-pair reagents, organic solvents and column temperature on the determination method were investigated and the retention rules discussed. Results found that TEA could be successfully analyzed by using 0.7 mmol/L 4-aminophenol hydrochloride and 0.15 mmol/L 1-heptanesulfonic acid sodium mixed with 20% （v/v） methanol as mobile phase at a UV detection wavelength of 230 nm. Under these conditions, the retention time of tetraethyl ammonium was 2.85 min. The detection limit （S/N = 3） for TEA was 0.06 mg/L. The relative standard deviations （n = 5） for peak area and retention time were 0.35% and 0.02%, respectively. The method has been successfully applied to the determination of synthesized tetraethyl ammonium bromide. Recovery of tetraethyl ammonium after spiking was 99.1%.
