Session: Advances in Mass Spectrometry:

The design of new and optimization of existing heterogeneous catalysts is of prime importance to progress the sustainable development of green, mild and effective depolymerisation and chemical modification strategies for the production of lignin-based chemicals and materials. For that purpose porous γ-Al₂O₃ supports have been examined extensively. Moreover, in order to improve porous γ-Al₂O₃ catalytic properties incorporation of different metallic nanoparticles (e.g., Pd, Pt, Ni, Fe, Cu) with synergistic catalytic activity is studied. In academia, researchers typically focus on alumina powders. In industry, however, macroscopically shaped supports such as microspheres, are preferred as they result in lower pressure drops when applied in a continuous flow reactor or can be more straightforward recovered from a batch reactor. As a result, characterization of nanoparticles incorporated in porous γ-Al₂O₃ microspheres is one of the topics of high interest for the transition from lab scale experimentation towards industrial scale production. The current state of the art techniques for characterizations of nanoparticles incorporated in porous γ-Al₂O₃ microspheres include SEM, EDX, FTIR, and XRD. However, complementary techniques might be required.
The goal of this research project is to develop novel methods using a carefully selected set of analytical tools for fast characterization and of metallic nanoparticles incorporated in porous γ-Al₂O₃. Herein, a novel sample preparation method and use of high resolution inductively coupled plasma-mass spectrometry operated in single-event mode (HR-spICP-MS; Nu AttoM ES, Nu Instruments, UK) for the fast and reliable characterization of Fe and Cu nanoparticles immobilized on porous γ-Al₂O₃ microspheres for synergistic catalytic activity for the reductive depolymerization of lignin is offered. More precisely, sample preparation includes mechanical milling of the microspheres for 5 minutes, followed by addition of Milli-Q water and mechanical milling of 10 min. The sample is sonicated for 30 min and finally dispersed in surfactant solution. HR-spICP-MS was performed after sample dilution in Milli-Q water providing information on the particle number density, size, size distribution, and the dimensional characterization.

Kristof Tirez

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