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A Photoreactor-Interfaced Mass Spectrometer: An Online Platform to Monitor Photochemical Reactions.
Oisin J Shiels1, Maria Menti-Platten1, Fostino R B Bokosi1
1Molecular Horizons and School of Chemistry and Molecular Bioscience, University of Wollongong, Wollongong NSW 2522, Australia.
Analytical Chemistry
|October 13, 2023
Summary
A new experimental platform enables real-time analysis of photochemical reactions using a continuous flow photoreactor coupled to a mass spectrometer. This system rapidly characterizes photopolymerization and photocatalyzed reactions, aiding mechanistic studies.
Area of Science:
- Analytical Chemistry
- Photochemistry
- Chemical Engineering
Background:
- Characterizing photochemical reactions often requires offline analysis, which can be time-consuming and may miss transient intermediates.
- Developing integrated systems for online monitoring of photoreactions is crucial for efficient reaction optimization and mechanistic elucidation.
Purpose of the Study:
- To report a novel experimental platform for the online characterization of photochemical reactions.
- To demonstrate the platform's capability in analyzing diverse photoreactions in real-time.
Main Methods:
- Coupling a continuous flow photoreactor with LED irradiation and a dual-electrospray ionization (ESI) source directly to a mass spectrometer.
- Utilizing electrospray ionization mass spectrometry (ESI-MS) for online detection and analysis.
- Applying the platform to study photopolymerization and photocatalyzed alkyne insertion reactions.
Main Results:
- The integrated system successfully performed online characterization of methyl methacrylate photopolymerization.
- The platform effectively monitored photocatalyzed alkyne insertion into 1,2,3-benzotriazinone.
- Real-time data acquisition provided rapid insights into reaction mechanisms and overall photochemistry.
Conclusions:
- The developed online platform offers a powerful tool for rapid and comprehensive characterization of photochemical reactions.
- This integrated approach accelerates the understanding of photochemical processes and facilitates reaction optimization.
- The system's versatility is demonstrated across different classes of photoreactions.

