Arkema Inc., King of Prussia, PA 19406, USA.
J Sep Sci. 2010 Jun;33(10):1480-6. doi: 10.1002/jssc.201000009.
2-D chromatography has become an important tool for the polymer chemist and engineer interested in understanding reaction mechanisms in multiple step polymerization reactions and for establishing the relationships between structure and property. As with 1-D chromatography, it is desirable to obtain the best possible resolution in order to distinguish subtle differences in composition and molecular weight. This requirement is in conflict with the need to keep the duration of the experiment short enough for practical purposes. In this paper, we use a model system to investigate the optimum conditions for improved 2-D resolution with a focus on the molecular weight dimension. This dimension is usually the less resolved in 2-D systems due to synchronization requirements between the two separation processes and the subsequent need to use a rapid size exclusion chromatography column. The method described here provides resolution in the SEC dimension equivalent to that of a standard 1-D SEC method, while maintaining a relatively short analysis time. Finally, a multi-angle light scattering detector was used to determine the radius of gyration of the eluting polymer.
二维色谱已成为对多步聚合反应的反应机制感兴趣的高分子化学家和工程师的重要工具，也有助于建立结构与性能之间的关系。与一维色谱一样，为了区分组成和分子量的细微差异，获得尽可能好的分辨率是很有必要的。这种要求与为了实际目的而保持实验持续时间足够短的需求相冲突。在本文中，我们使用模型体系研究了提高二维分辨率的最佳条件，重点是分子量维度。由于两个分离过程之间的同步要求以及随后需要使用快速尺寸排阻色谱柱，在二维系统中，这个维度通常分辨率较低。这里描述的方法在 SEC 维度上提供了与标准一维 SEC 方法相当的分辨率，同时保持相对较短的分析时间。最后，使用多角度光散射检测器来确定洗脱聚合物的回转半径。
