Core R&D Analytical Sciences, The Dow Chemical Company, Spring House, PA 19477-0904, USA.
J Sep Sci. 2013 Sep;36(17):2718-27. doi: 10.1002/jssc.201300444. Epub 2013 Aug 2.
Ultra-high performance size-exclusion chromatography (UHP SEC) is a newly developed disruptive technology that allows the high-resolution separation of synthetic polymers in as little as 2 min. The capability of UHP SEC for the characterization of synthetic polymers in organic solvents has been demonstrated. Using the Waters ACQUITY UPLC® H-Class system and ethylene-bridged hybrid size-exclusion chromatography (SEC) columns packed with 1.7 to 2.5-μm particles with pore sizes ranging from 45 to 900 Å, size-based separations of polystyrene and poly(methyl methacrylate) standards in tetrahydrofuran and poly(ethylene oxide) standards in 20 mM ammonium acetate in methanol are achieved within 2-4 min. The speed of analysis is about ten times faster than conventional SEC separations, and greater resolution is achieved. Average molecular weights of selected commercial polymers have been determined using ultra-high performance and conventional SEC. Average M data of analyzed samples are in good agreement using the two approaches. An inherent limitation of SEC in UHP mode is the characterization of very high M polymers (above ca. 2 million Da) due to the deformation and/or mechanical shearing of large molecules at high flow rates.
超高效体积排阻色谱（UHP SEC）是一种新兴的颠覆性技术，它可以在短短 2 分钟内实现合成聚合物的高分辨率分离。UHP SEC 已经证明了其在有机溶剂中对合成聚合物进行表征的能力。使用沃特世 ACQUITY UPLC® H-Class 系统和填充有 1.7 至 2.5μm 粒径、孔径范围为 45 至 900Å 的乙撑桥接混合体积排阻色谱（SEC）柱，在四氢呋喃中实现了聚苯乙烯和聚甲基丙烯酸甲酯标准品以及在甲醇中的 20 mM 乙酸铵中的聚氧化乙烯标准品的基于尺寸的分离，在 2-4 分钟内即可完成。分析速度比传统 SEC 分离快约十倍，并且实现了更高的分辨率。使用超高效和常规 SEC 确定了选定商业聚合物的平均分子量。使用两种方法分析的样品的平均 M 数据吻合良好。UHP 模式下 SEC 的一个固有局限性是对非常高分子量聚合物（高于约 200 万 Da）的表征，因为在高流速下大分子会发生变形和/或机械剪切。
