Comprehensive two-dimensional liquid chromatography for the characterization of functional acrylate polymers
Comprehensive two-dimensional liquid chromatography for the characterization of functional acrylate polymers
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DOI：
10.1016/j.chroma.2005.03.135
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发表时间：
2005-05-27
影响因子：
4.1
通讯作者：
Schoenmakers, PJ
中科院分区：
文献类型：
--
作者：
Jiang, XL;van der Horst, A;Schoenmakers, PJ
研究了全二维液相色谱-尺寸排阻色谱(LC-SEC)作为表征功能聚甲基丙烯酸甲酯(PMMA)聚合物的工具。采用紫外吸收和蒸发光散射检测(ELSD)。提出了一种对ELSD数据进行量化的简单方法。ELSD色谱图中的每个数据点都可以使用实验校准曲线转换为质量浓度。在两个代表性样品上获得的定性和定量信息被用来证明LC x SEC在确定功能聚合物的相互依赖的摩尔质量分布(MMD)和官能度类型分布(FTD)方面的适用性。用LC-X-SEC研究了羟基功能PMMA聚合物在LC中的保留行为，考察了摩尔质量对保留行为的影响。根据定义，保留率与摩尔质量无关的临界条件对于具有不同端基的PMMA系列并不完全相同。我们的观察结果与文献报道的理论曲线非常一致。然而，对于LC x SEC的实际应用，并不是严格需要在精确的临界溶剂组成下工作。近临界条件通常足以确定功能聚合物的相互依赖分布(MMD和FTD)。(C)2005 Elsevier B.V.保留所有权利。
Comprehensive two-dimensional liquid chromatography-size-exclusion chromatography (LC x SEC) was investigated as a tool for the characterization of functional poly(methyl methacrylate) (PMMA) polymers. Ultraviolet-absorbance and evaporative light-scattering detection (ELSD) were used. A simple method to quantify ELSD data is presented. Each data point from the ELSD chromatogram can be converted into a mass concentration using experimental calibration curves. The qualitative and quantitative information obtained on two representative samples is used to demonstrate the applicability of LC x SEC for determining the mutually dependent molar-mass distributions (MMD) and functionality-type distributions (FTD) of functional polymers. The influence of the molar mass on the retention behavior in LC was investigated using LC x SEC for hydroxyl-functional PMMA polymers. The critical conditions, at which retention is - by definition - independent of molar mass, were not exactly the same for PMMA series with different end-groups. Our observations are in close agreement with theoretical curves reported in the literature. However, for practical applications of LC x SEC it is not strictly necessary to work at the exact critical solvent composition. Near-critical conditions are often sufficient to determine the mutually dependent distributions (MMD and FTD) of functional polymers. (c) 2005 Elsevier B.V. All rights reserved.