Robust isocratic liquid chromatographic separation of functional poly(methyl methacrylate).
Robust isocratic liquid chromatographic separation of functional poly(methyl methacrylate).
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DOI：
10.1016/j.chroma.2003.08.035
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发表时间：
2003-11
期刊：
影响因子：
--
通讯作者：
Xulin Jiang;V. Lima;P. Schoenmakers
中科院分区：
文献类型：
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作者：
Xulin Jiang;V. Lima;P. Schoenmakers
本文研究了在临界液相色谱条件下，利用能与极性官能团相互作用的裸硅胶柱，基于端基数目分离遥爪聚甲基丙烯酸甲酯（PMMA）预聚物。在正相LC中，使用不同组成的乙腈和二氯甲烷（DCM）的混合物作为移动的相，确定了非官能、单官能和双官能PMMA的临界溶剂组成。在临界条件下，根据羟基（OH）官能度（分别具有零，一个或两个OH基团）成功地分离了遥爪预聚物，其中快速（5分钟），基线分离独立于分子量。在一定范围内改变柱温、流速和流动相组成对功能性分离没有影响。因此，该等度LC分离方法相当耐用。蒸发光散射检测器（ELSD）校准曲线用于定量分析的功能PMMA预聚物。
The separation of telechelic poly(methyl methacrylate) (PMMA) prepolymers based on the number of end-groups under critical liquid chromatography (LC) conditions has been studied using a bare-silica column, which can interact with polar functional groups. The critical solvent compositions for non-functional, mono-functional and bi-functional PMMAs were determined in normal-phase LC using mixtures of acetonitrile and dichloromethane (DCM) of varying composition as the mobile phase. The telechelic prepolymers were successfully separated according to hydroxyl (OH) functionality (with zero, one, or two OH groups, respectively) under the critical conditions, in which fast (5min), base-line separations were obtained independent of molecular weight. Changing the column temperature, flow rate, and mobile-phase composition within a certain range did not affect the functionality separation. Therefore this isocratic LC separation method is quite robust. Evaporative light-scattering detector (ELSD) calibration curves were used for the quantitative analysis of functional PMMA prepolymers.