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Data Processing Method for the Determination of Accurate Molecular Weight Distribution of Polymers by SEC/MALDI-MS

机译:SEC / MALDI-MS测定聚合物准确分子量分布的数据处理方法

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摘要

A novel data processing method for a hyphenated technique, size exclusion chromatography/matrix-assisted laser desorption/ionization-mass spectrometry (SEC/MALDI-MS), has been proposed to determine accurate molecular weight distributions on the basis of the individual oligomer species of a polymer. This method is based on the concept that the individual peak intensities of MALDI mass spectrum observed for every SEC fraction with narrow molecular weight distribution could be adjusted to the quantified values to reveal the accurate molecular weight distribution using the signal intensity of the corresponding fraction on the SEC chromatogram observed with a refractive index detector. At first, the theory of the proposed date processing is described in detail. Then, experimental verification of the method is described. This was performed through the characterization of mixtures of three kinds of monodispersed polystyrene reference materials (weight average molecular weight = ca. 6000, 10000, and 18000) as model samples. An accurate trimodal molecular weight distribution for the individual oligomer species of the sample was obtained without any influence of the chromatographic band broadening observed in the original SEC chromatogram. Moreover, the method for depicting the elution profiles of individual oligomer species during SEC separation was also obtained as a “mass chromatogram” using the data processing procedure.
机译:提出了一种用于连接技术的新型数据处理方法,即尺寸排阻色谱法/基质辅助激光解吸/电离质谱法(SEC / MALDI-MS),可根据单个低聚物的分子量确定准确的分子量分布。聚合物。该方法基于以下概念:可以将分子量分布窄的每个SEC馏分观察到的MALDI质谱的单个峰强度调整为定量值,以使用色谱柱上相应馏分的信号强度显示准确的分子量分布。用折射率检测器观察到的SEC色谱图。首先,详细描述提出的日期处理的理论。然后,描述了该方法的实验验证。这是通过表征三种单分散聚苯乙烯参考材料(重均分子量=约6000、10000和18000)作为模型样品的混合物来进行的。在不影响原始SEC色谱图中观察到的色谱带展宽的情况下,获得了样品中各个低聚物种类的准确三峰分子量分布。此外,还使用数据处理程序获得了描述SEC分离过程中单个低聚物物种洗脱曲线的方法,以“质谱图”的形式获得。

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