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Novel fabrication of on-column capillary inlet frits through flame induced sintering of stainless steel particles

机译:通过火焰诱导的不锈钢颗粒烧结来新型制备柱上毛细管入口玻璃料

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A novel fritting technology was introduced for the fused-silica capillary. The technique involved sintering of stainless steel (SS) particles at the tip of capillary through flame heating. A simple butane gas based welding torch was used for sintering the SS particles. The new fritting technique, flame induced sintering of SS particles (FIS/SSP), was applied for making frits with different inlet diameters (75 mu m, 100 mu m, 250 mu m and 530 mu m). The changes in morphologies of SS particles during sintering process were identified by scanning electron microscopy (SEM). Frits with the length of 0.5-1 mm and capillaries with inner diameter about 50-100 mu m were fabricated through suitable selection of experimental conditions (size of SS particles and heating mode). The frits prepared by FIS/SSP technique exhibited adequate separation properties and mechanical strength. Columns packed with C-18 particles were stable with these frits in a few important chromatographic operations. Frits prepared by FIS/SSP technique was used in three typical separation modes namely, capillary electrochromatography (CEC), p-assisted CEC (p-CEC) and low pressure liquid chromatography (LPLC). Importantly, no bubble formation was noticed with the frit over a period of one week. A good peak symmetry and high efficiency for separation were obtained using pressure-assisted CEC, p-CEC and low pressure-driven separation modes.
机译:一种用于熔融石英毛细管的新型熔结技术被引入。该技术涉及通过火焰加热在毛细管尖端烧结不锈钢(SS)颗粒。使用简单的基于丁烷气的焊炬烧结SS颗粒。新型烧结技术,即火焰诱导的SS颗粒烧结(FIS / SSP),被用于制造具有不同入口直径(75μm,100μm,250μm和530μm)的玻璃料。通过扫描电子显微镜(SEM)鉴定了SS颗粒在烧结过程中的形态变化。通过适当选择实验条件(SS颗粒的大小和加热方式),可以制成长度为0.5-1 mm的玻璃料和内径为50-100μm的毛细管。用FIS / SSP技术制备的玻璃料具有足够的分离性能和机械强度。在一些重要的色谱操作中,用C-18颗粒填充的色谱柱对这些玻璃料稳定。通过FIS / SSP技术制备的玻璃料用于三种典型的分离模式,即毛细管电色谱(CEC),p辅助CEC(p-CEC)和低压液相色谱(LPLC)。重要的是,在一周内没有观察到熔块形成气泡。使用压力辅助CEC,p-CEC和低压驱动的分离模式可获得良好的峰对称性和高分离效率。

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