Benchtop ¹H and ¹⁹F NMR as an analytical tool for monitoring photocatalytic degradation
Abstract
Background: Reliable monitoring of photocatalytic degradation requires analytical techniques capable of delivering selective and molecular-level information. In this study, low-field benchtop NMR spectroscopy is evaluated as an accessible tool for monitoring the degradation of model pollutants under LED irradiation at 371 nm using supported TiO₂ photocatalysts. Results: A dedicated LED–NMR setup was developed to enable both ex situ and in situ UV irradiation within a 60 MHz NMR spectrometer using TiO₂-coated quartz rods. The effective NMR detection zone was experimentally defined to prevent magnetic perturbations induced by solid inserts, and experimental parameters were evaluated to ensure adequate signal-to-noise ratio tailored to both time-limited acquisition and millimolar-scale reaction monitoring. Both ¹H and ¹⁹F nuclei were investigated, enabling complementary monitoring of protonated and fluorinated species. Conclusion: The analytical performance of the method was assessed using three representative model pollutants: methylene blue (MB), 5-fluorouracil (5-FU), and perfluorooctanoic acid (PFOA). Benchtop NMR enabled reproducible monitoring of degradation profiles, detection of transformation products, and differentiation between adsorption phenomena and photolysis. These results demonstrate that LED-assisted benchtop NMR constitutes a valuable proof-of-concept for the in situ monitoring of model photocatalytic processes
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BibTeX
@article{pujol2026benchtop,
title = {{Benchtop ¹H and ¹⁹F NMR as an analytical tool for monitoring photocatalytic degradation}},
author = {Camille Pujol and Véronique Gilard and Florence Benoît-Marquié and Stéphane Balayssac},
journal = {Analytica Chimica Acta},
year = {2026},
month = oct,
doi = {10.1016/j.aca.2026.345863},
url = {https://hal.science/hal-05687149v1},
note = {CC BY 4.0},
}
RIS
TY - JOUR
TI - Benchtop ¹H and ¹⁹F NMR as an analytical tool for monitoring photocatalytic degradation
AU - Camille Pujol
AU - Véronique Gilard
AU - Florence Benoît-Marquié
AU - Stéphane Balayssac
PY - 2026
DA - 2026/10/09
JO - Analytica Chimica Acta
DO - 10.1016/j.aca.2026.345863
UR - https://hal.science/hal-05687149v1
AB - Background: Reliable monitoring of photocatalytic degradation requires analytical techniques capable of delivering selective and molecular-level information. In this study, low-field benchtop NMR spectroscopy is evaluated as an accessible tool for monitoring the degradation of model pollutants under LED irradiation at 371 nm using supported TiO₂ photocatalysts. Results: A dedicated LED–NMR setup was developed to enable both ex situ and in situ UV irradiation within a 60 MHz NMR spectrometer using TiO₂-coated quartz rods. The effective NMR detection zone was experimentally defined to prevent magnetic perturbations induced by solid inserts, and experimental parameters were evaluated to ensure adequate signal-to-noise ratio tailored to both time-limited acquisition and millimolar-scale reaction monitoring. Both ¹H and ¹⁹F nuclei were investigated, enabling complementary monitoring of protonated and fluorinated species. Conclusion: The analytical performance of the method was assessed using three representative model pollutants: methylene blue (MB), 5-fluorouracil (5-FU), and perfluorooctanoic acid (PFOA). Benchtop NMR enabled reproducible monitoring of degradation profiles, detection of transformation products, and differentiation between adsorption phenomena and photolysis. These results demonstrate that LED-assisted benchtop NMR constitutes a valuable proof-of-concept for the in situ monitoring of model photocatalytic processes
SN - 0003-2670
ER -