Characterization of ultrahigh molecular weight poly(ethylene oxide) by size-exclusion chromatography with multiangle light scattering detection

回转半径 分散性 化学 大小排阻色谱法 多角度光散射 分析化学(期刊) 校准曲线 环氧乙烷 色谱法 摩尔质量分布 聚合物 光散射 检出限 散射 光学 高分子化学 共聚物 物理 有机化学 生物化学
作者
Dean Lee,Yucheng Zhu,Byeong Chae,Elizabeth J Tocce
出处
期刊:Journal of Chromatography A [Elsevier]
卷期号:1659: 462640-462640 被引量:4
标识
DOI:10.1016/j.chroma.2021.462640
摘要

This study investigated the experimental conditions needed to obtain molecular weight distribution (MWD) of ultrahigh MW poly(ethylene oxide) (PEO) using size exclusion chromatography (SEC) hyphenated with a multiangle light scattering photometer (MALS) and a differential refractive index detector (RI). Ultrahigh MW components yielded non-linear angular dependency in scattered light intensities. The first-order linear fitting using Zimm formalism resulted in significant differences in MW depending on if the signals from detector 4 to 16 were used in the fitting or only five low-angles from 4 to 8 were used. In contrast, no significant differences in MW were obtained for lower MW PEO samples (equal or less than 1000 KDa) between the two fitting approaches. It was thus proposed to use only the five low-angles to derive MW for a sample with broad polydispersity including both ultrahigh and low MW components. The SEC separation was done using one column designed for ultrahigh MW polymer separation connected with another mixed-bed column. The ultrahigh MW column allowed separation and characterization of polymeric components in the MW range between 10 and 50 million Dalton (MDa) and the size range between 300 and 600 nm in radius of gyration (Rg). Online calibration curves were obtained from the linear fittings of MW as a function of elution volume. MW polydispersity was derived from the online calibration curve showing that the ultrahigh MW PEO had higher polydispersity than the lower MW samples. The double logarithmic plot of radius of gyration versus MW indicated that both ultrahigh MW and low MW PEO would adopt expanded coil conformations in the aqueous solution.
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