Kinetic investigation of narrow-bore columns packed with prototype sub-2 μm superficially porous particles with various shell thickness
Kinetic investigation of narrow-bore columns packed with prototype sub-2 μm superficially porous particles with various shell thickness
复制标题
DOI：
10.1016/j.chroma.2011.07.037
复制
发表时间：
2011-10-07
影响因子：
4.1
通讯作者：
Guiochon, Georges
中科院分区：
文献类型：
--
作者：
Gritti, Fabrice;Omamogho, Jesse;Guiochon, Georges
最近 HPLC 中亚 3 μm 壳颗粒的成功突破引发了针对新品牌核壳颗粒设计的大量研究工作。我们研究了一些分析物在填充有原型 1.7 μm 壳颗粒的窄孔柱中的传质机制，这些颗粒由 1.0、1.2 和 1.4 μm 固体无孔核组成，周围分别被厚度为 350、250 和 150 nm 的多孔壳包围。选择三种探针溶质：尿嘧啶、萘和胰岛素来评估这些柱的动力学性能。进行反尺寸排阻色谱、峰停放实验和实验峰轮廓的数值积分，以测量外部、内部和总柱孔隙率、这些分析物的真实体积扩散系数、相当于理论塔板的高度、纵向扩散项和跨颗粒传质阻力项。通过差值测量残余涡流扩散项。结果表明，存在重要的跨柱速度偏差（7%），这可能是由于填充过程中使用的浆料混合物中存在多重粒子所致。我们的结果说明了科学家在制备壳颗粒并将其填充到窄孔柱中时遇到的一些困难。 (C) 2011 Elsevier B.V. 保留所有权利。
The recent successful breakthrough of sub-3 mu m shell particles in HPLC has triggered considerable research efforts toward the design of new brands of core-shell particles. We investigated the mass transfer mechanism of a few analytes in narrow-bore columns packed with prototype 1.7 mu m shell particles, made of 1.0, 1.2, and 1.4 mu m solid nonporous cores surrounded by porous shells 350, 250, and 150 nm thick, respectively. Three probe solutes, uracil, naphthalene, and insulin, were chosen to assess the kinetic performance of these columns. Inverse size exclusion chromatography, peak parking experiments, and the numerical integration of the experimental peak profiles were carried out in order to measure the external, internal, and total column porosities, the true bulk diffusion coefficients of these analytes, the height equivalent to a theoretical plate, the longitudinal diffusion term, and the trans-particle mass transfer resistance term. The residual eddy diffusion term was measured by difference. The results show the existence of important trans-column velocity biases (7%) possibly due to the presence of particle multiplets in the slurry mixture used during the packing process. Our results illustrates some of the difficulties encountered by scientists preparing and packing shell particles into narrow-bore columns. (C) 2011 Elsevier B.V. All rights reserved.