Analytical Laboratory, Department of Chemistry, Konkuk University, 1 Hwayangdong, Gwangjingu, Seoul 143-701, South Korea.
J Chromatogr A. 2011 Oct 28;1218(43):7895-9. doi: 10.1016/j.chroma.2011.08.097. Epub 2011 Sep 9.
A simple but effective frit formation technique was developed to stabilize the packing structure inside the microchannel of capillary electrochromatographic microchips, utilizing the electroless plating technique. A Ag(NH(3))(2)(+) solution was allowed to diffuse through the colloidal silica packing in the microchannel from the reservoir of the microchip for a limited amount of time, and then it was reduced by an excess amount of formaldehyde solution. A frit structure of ~70 μm in length was formed at the entrance of the microchannel without clogging when treated with 1mM Ag(NH(3))(2)(+) ion and formaldehyde for 30s and 150 s, respectively. The formation of the frit structure was confirmed by a scanning electron microscopy. The stability of the packing structure was tested rigorously and then confirmed by applying alternating electroosmotic flows back and forth with pulsed potential steps on both sides of the frit structure. The effect of the treatment on the electrochromatograms was evaluated after the microchips were repeatedly used and stored for a long period of time. The results indicated that the silver-cemented frit structure extended the lifetime of the fully packed CEC microchips distinctly.
开发了一种简单有效的 frit 形成技术,利用化学镀技术来稳定毛细管电色谱微芯片微通道内的填充结构。将 Ag(NH(3))(2)(+)溶液允许在有限的时间内从微芯片的储液器扩散通过微通道中的胶体二氧化硅填充,然后用过量的甲醛溶液还原。当用 1mM Ag(NH(3))(2)(+)离子和甲醛分别处理 30s 和 150s 时,在微通道入口处形成了长度约为 70μm 的 frit 结构,而不会堵塞。通过扫描电子显微镜确认了 frit 结构的形成。通过在 frit 结构两侧施加交替的电渗流和脉冲电势步长来严格测试填充结构的稳定性,并对其进行了确认。在微芯片被反复使用和长时间储存后,评估了处理对电色谱图的影响。结果表明,银固结的 frit 结构明显延长了完全填充的 CEC 微芯片的寿命。