Yao Yan, Lenhoff Abraham M
Department of Chemical Engineering, University of Delaware, Newark, DE 19716, USA.
J Chromatogr A. 2004 May 28;1037(1-2):273-82. doi: 10.1016/j.chroma.2004.02.054.
The macroscopic properties of porous chromatographic adsorbents are directly influenced by the pore structure, with the pore size distribution (PSD) playing a major role beyond simply the mean pore size. Inverse size-exclusion chromatography (ISEC), a widely used chromatographic method for determining the PSD of porous media, provides more relevant information on liquid chromatographic materials in situ than traditional methods, such as gas sorption and mercury intrusion. The fundamentals and applications of ISEC in the characterization of the pore structure are reviewed. The description of the probe solutes and the pore space, as well as theoretical models for deriving the PSD from solute partitioning behavior, are discussed. Precautions to ensure integrity of the experiments are also outlined, including accounting for probe polydispersity and minimization of solute-adsorbent interactions. The results that emerge are necessarily model-dependent, but ISEC nonetheless represents a powerful and non-destructive source of quantitative pore structure information that can help to elucidate chromatographic performance observations covering both retention and rate aspects.
多孔色谱吸附剂的宏观性质直接受孔隙结构影响，孔径分布（PSD）所起的作用不仅限于平均孔径，还至关重要。反相尺寸排阻色谱法（ISEC）是一种广泛用于测定多孔介质PSD的色谱方法，与传统方法（如气体吸附和压汞法）相比，它能原位提供更多关于液相色谱材料的相关信息。本文综述了ISEC在孔隙结构表征方面的基本原理和应用。讨论了探针溶质和孔隙空间的描述，以及从溶质分配行为推导PSD的理论模型。还概述了确保实验完整性的注意事项，包括考虑探针的多分散性以及尽量减少溶质与吸附剂的相互作用。所得结果必然依赖于模型，但ISEC仍然是定量孔隙结构信息的强大且无损的来源，有助于阐明涵盖保留和速率方面的色谱性能观察结果。
