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Polymer Analysis by Micro-Scale Size-Exclusion Chromatography/MALDI Time-of. Flight Mass Spectrometry with a Robotic Interface

机译:通过微尺度尺寸排阻色谱法/ MALDI-time进行聚合物分析。具有机械手界面的飞行质谱

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摘要

Polydisperse synthetic polymers cannot be characterized ,reliably by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MAL1H MS) alone. Coupling of size-exclusion chromatography (SEC) with MALDI MS provides both absolute mass calibration of the SEC column based on the polymer itself and determination of monomers and end groups from the mass spectra. Now a micro-scale SEC μSEC) system has been developed in which the MALDI matrix solution is coaxially added to the column effluent and directly spotted onto the MALDI targets in a robotic interface. Each spot corresponds with a lO-s elution window from the μSEC column, thus yielding a narrow polymer distribution which is amenable to characterization by MALDI MS. This μSEC/MALDI MS system is less laborious and time-consuming and features very low solvent consumption and reduced solvent emission during the evaporation step as compared to the conventional-sized SEC/fraction collector systems applied in the past. The performance is demon-mated by the characterization of a polybisphenol A carbonate and a complex dipropoxylated bisphenol A/adipic acid/isophthalic acid copolyester resin.
机译:仅靠基质辅助激光解吸/电离飞行时间质谱(MAL1H MS)不能可靠地表征多分散合成聚合物。尺寸排阻色谱(SEC)与MALDI MS的偶联提供了基于聚合物本身的SEC色谱柱绝对质量校准以及从质谱确定单体和端基的功能。现在,已开发出一种微型SEC(SEC)系统,其中将MALDI基质溶液同轴添加到色谱柱流出物中,并通过机械手界面直接点样到MALDI目标上。每个斑点对应于来自μSEC色谱柱的10s洗脱窗口,因此产生的聚合物分布窄,可以通过MALDI MS表征。与过去使用的常规尺寸的SEC /馏分收集器系统相比,该μSEC/ MALDI MS系统省时省力,并且在蒸发步骤中具有极低的溶剂消耗并减少了溶剂排放。该性能通过多双酚A碳酸酯和复合双丙氧基化双酚A /己二酸/间苯二甲酸共聚酯树脂的表征来证明。

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