Development of Hyphenated Analytical Instruments for Speciation analysis for Trace Elements

制备了各种聚甲基丙烯酸酯基毛细管整体柱，用于微型HPLC-ICP-MS和CEC-ICP-MS联用仪器的开发。熔融石英毛细管和随后的基于环氧化物与1M Na_2SO_3开环的磺化。用Na ^+、NH 4 ^+、K ^+、Mg ^2+、Ca ^2+等常见阳离子评价了柱的色谱性能。例如，它们可以在容量为0.15毫当量/毫升的15厘米柱上彼此很好地分离，其中该15厘米柱的压降为约1.5毫当量/毫升。1MPa，在1 mm/s的法向线速度（3 μ L/min的流速）下，阳离子的理论板数大于3000板/15 cm。此外，该柱可以承受至少10 mm/s的高线性速度。这种基于GMA的方法被扩展到强阴离子交换柱的制备，其中季铵基团被引入由开环反应的环氧化物与烷基胺化合物，然后与苄基或烷基卤化物的反应。反相柱也制备了各种甲基丙烯酸烷基酯和乙二醇二甲基丙烯酸酯的自由基聚合。此外，还使用这种基于GMA的方法开发了显示反相分离模式的CEC柱。

Various types of polymethacrylate-based monolithic capillary columns were newly prepared for the development of hyphenated instruments such as micro-HPLC-ICP-MS and CEC-ICP-MS. Strong cation-exchange monolithic capillary columns were constructed for ion chromotography by radical polymerization of glycidyl methacrylate (GMA) and ethylene dimethacrylate in a 250-μm-i.d. fused silica capillary and its subsequent sulfonatiori based on ring opening of epoxides with 1 M Na_2SO_3. The chromotographic performance of the columns was evaluated through common cations such as Na^+,NH_4^+,K^+,Mg^<2+> and Ca^<2+>. For an example, they could be well separated from one another on a 15 cm column with a capacity of 0.15 mequiv/mL where the pressure drop of this 15 cm column was ca. 1 MPa at a normal linear velocity of 1 mm/s (a flow rate of 3 μL/min) and the number of theoretical plates for the cations was above 3000 plates/15 cm. Moreover, this column could withstand high linear velocities of at least 10 mm/s. This GMA-based approach was extended to the preparation of strong anion-exchange columns where quaternary ammonium groups were introduced by the ring opening reaction of the epoxides with alkylamine compounds followed by the reaction with benzyl or alkyl halides. Reversed-phase columns were also prepared by radical polymerization of various alkyl methacrylates and ethylene glycol dimethacrylate. Moreover, CEC columns which show reversed-phase separation modes were also developed with this GMA-based approach.