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Article Dans Une Revue Analytical Chemistry Année : 2021

Determination of Photoinduced Radical Generation Quantum Efficiencies by Combining Chemical Actinometry and 19 F NMR Spectroscopy

Jean Rouillon
Caroline Arnoux
  • Fonction : Auteur
Cyrille Monnereau

Résumé

We introduce a general and relatively straightforward protocol aimed at determining the absolute photoinduced radical generation efficiency via NMR monitoring. This approach relies on the use of a radical scavenger probe that combines a nitroxide moiety that specifically reacts with radicals, and a trifluoromethyl group used as a 19 F NMR signaling unit. Using a LED source, which fluence is precisely determined by a chemical actinometry procedure also described herein, the method is used to determine the radical photogeneration quantum yields of three well-known polymerization initiators: Azobisisobutyronitrile (AIBN), 4,4'-Bis(N,N-diethylamino)benzophenone (BDEBP, a derivative of Michler's ethyl ketone) and 2,4,6-trimethylbenzoyl diphenylphosphine oxide (MAPO). The overall good agreement with values previously reported in the literature proves the robustness of this new method. We then extended the study to the precise measurement of the quantum yield of free-radical photogeneration of a newly synthesized photoinitiator used for two-photon direct laser writing. This paper highlights the potential of this methodology for the quantitative determination of photoinduced radical generation efficiency used in many fields of applications.
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Dates et versions

hal-03590669 , version 1 (28-02-2022)

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Jean Rouillon, Caroline Arnoux, Cyrille Monnereau. Determination of Photoinduced Radical Generation Quantum Efficiencies by Combining Chemical Actinometry and 19 F NMR Spectroscopy. Analytical Chemistry, 2021, 93 (5), pp.2926-2932. ⟨10.1021/acs.analchem.0c04540⟩. ⟨hal-03590669⟩
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