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.
Keywords: end group analysis; online coupling; quantum cascade laser infrared spectroscopy (QCL-IR); size-exclusion chromatography (SEC).
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