A New Quantum Cascade IR-Laser Online Detector: Chemical-Sensitive Size-Exclusion Chromatography Measurement at Unprecedented Low Levels.

ABSTRACT

Online chemically sensitive detectors for size exclusion chromatography (SEC) through coupled setups based on infrared (IR) (or NMR) spectrometers present new possibilities through unprecedented levels of polymer detail with respect to molecular weight and chemical composition. Herein, a new external cavity quantum cascade laser (EC-QCL) mid-IR spectrometer as a chemically sensitive online detector for SEC is custom-designed, built, and tested. This unique spectrometer features multiple broadly tunable EC-QCL sources, which can be operated in continuous wave and pulsed mode, accompanied with balanced liquid nitrogen cooled mercury cadmium telluride (MCT) detectors and a new custom-built transmission flow cell. Automated data analysis is done with a self-written MATLAB code. The limit of detection (LOD) is measured online, coupled with SEC chromatography, where on average, one carbonyl functionality in 530 000 g mol-1 at chromatographic conditions for SEC could be detected. It is possible to detect 0.46 µg (LOD) PMMA, which is approximately a factor of 30 lower than that reported for SEC-Fourier transform infrared.