Online Detection of Functional Groups in SEC via Quantum Cascade Laser IR Spectroscopy,Macromolecular Rapid Communications

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Online Detection of Functional Groups in SEC via Quantum Cascade Laser IR Spectroscopy
Macromolecular Rapid Communications ( IF 4.2 ) Pub Date : 2017-11-02 , DOI: 10.1002/marc.201700307
Sascha Morlock ₁ , Jennifer M. Kübel ₁ , Timo F. Beskers ₂ , Bernhard Lendl ₃ , Manfred Wilhelm ₁

Affiliation

The development of coupled techniques based on chemically sensitive detectors, such as FTIR or NMR spectrometers, for size exclusion chromatography (SEC) provides sophisticated methods for determining the molecular‐weight‐dependent chemical composition in polymers. However, the detection of rare functionalities such as end groups or branching points presents a challenge, especially for online coupled SEC detection, which is based on low‐concentration chromatography. To address this issue, for the first time, an external cavity quantum cascade laser (EC‐QCL) infrared spectrometer is coupled to an SEC. The system is evaluated using polystyrene/poly(methyl methacrylate) (PS/PMMA) blends. The current limit of detection for the carbonyl (PMMA) stretch vibration at 1730 cm⁻¹ with this technique is 3.5 µg PMMA on a semipreparative column (typical load of 2.5 mg polymer in total). That equals 0.15 mol% of PMMA in the PS/PMMA blend and corresponds to one carbonyl group per 70 kg mol⁻¹ polymer.

中文翻译：

通过量子级联激光红外光谱在线检测SEC中的官能团

基于化学敏感检测器（例如FTIR或NMR光谱仪）的尺寸排阻色谱（SEC）耦合技术的开发提供了用于确定聚合物中分子量依赖性化学组成的复杂方法。但是，检测稀有功能（例如端基或分支点）提出了挑战，尤其是对于基于低浓度色谱法的在线偶联SEC检测。为了解决这个问题，首次将外腔量子级联激光器（EC-QCL）红外光谱仪与SEC耦合。使用聚苯乙烯/聚（甲基丙烯酸甲酯）（PS / PMMA）混合物评估系统。羰基（PMMA）拉伸振动在1730 cm ^-1时的检测电流极限使用这种技术时，在半制备色谱柱上可得到3.5 µg PMMA（典型的总负载量为2.5 mg聚合物）。这等于在PS / PMMA共混物中的0.15mol％的PMMA，并且对应于每70kg mol ^-1聚合物一个羰基。

更新日期：2017-11-02

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