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使用高温尺寸排阻色谱法和高温非对称流场流分离法研究低密度聚乙烯在尺寸排阻色谱中的异常晚期共洗脱现象。

Study of the abnormal late co-elution phenomenon of low density polyethylene in size exclusion chromatography using high temperature size exclusion chromatography and high temperature asymmetrical flow field-flow fractionation.

机构信息

Postnova Analytics GmbH, Max-Planck-Straße 14, 86899 Landsberg/Lech, Germany.

出版信息

J Chromatogr A. 2011 Jul 8;1218(27):4240-8. doi: 10.1016/j.chroma.2011.01.009. Epub 2011 Jan 11.

Abstract

The elution behaviour of linear and branched polyethylene samples in SEC was studied. For the branched samples an abnormal late co-elution of large and small macromolecules manifests itself as an abnormal re-increase of the molar mass and the radius of gyration values detected with multi angle light scattering at high elution volumes in SEC. The late co-elution of small and large macromolecules cannot be explained by the SEC mechanism alone. The influence of several experimental parameters on the late co-elution was studied. It was found that the type of SEC column and the flow rate have a significant influence. The late eluting part of the sample was fractionated and separated by HT-SEC- and HT-AF4-MALS. The different results of both methods have been discussed with the aim to find possible explanations for the late elution. The experiments indicate that especially large branched structures show an increased tendency for the phenomenon.

摘要

研究了线性和支化聚乙烯样品在 SEC 中的洗脱行为。对于支化样品,大分子量和小分子量的大分子异常晚期共洗脱表现为在 SEC 高洗脱体积下多角光散射检测到的摩尔质量和回转半径值的异常再增加。仅用 SEC 机制无法解释小分子和大分子的晚期共洗脱。研究了几个实验参数对晚期共洗脱的影响。发现 SEC 柱的类型和流速有显著影响。通过 HT-SEC-和 HT-AF4-MALS 对样品的晚期洗脱部分进行了分级和分离。讨论了两种方法的不同结果,目的是为晚期洗脱找到可能的解释。实验表明,特别是大的支化结构表现出增加的趋势。

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