NMR-Analytics

Nuclear magnetic resonance (NMR) techniques have been established for years in the natural sciences (especially in synthetic chemistry) for the characterization of reaction mixtures. Structure elucidation and purity analysis are performed here as standard. In engineering sciences, the use of this method has so far been limited. In the LASE-MR group we use 1D and 2D NMR methods to characterize complex mixtures. In this way, product distributions from chemical reaction, chemical equilibria and phase equilibria are analyzed.

Characterization of Formaldehyde-Containing Systems

Formaldehyde is an important basic chemical in the chemical industry. The technical separation of mixtures containing formaldehyde is complex and non-trivial due to the high reactivity. The aim of our work is to gain an in-depth understanding of the complex material and reaction system of mixtures of formaldehyde with water and/or alcohols. Of great importance is the quantification of free, monomeric formaldehyde and the characterization of the Cannizzaro reaction as a side reaction in the reaction system by NMR experiments.

Figure: Schematic of the physicochemical model of the solid-liquid equilibrium in the system (formaldehyde + water + methanol).

Chemical Reactions in Cold Plasma

Reactions in cold plasma can open up new synthesis routes. In this project, the reaction of methane with oxygen is considered; synthesis gas and methanol, among others, are formed in a gas phase reaction in cold plasma in the range of room temperature at normal pressure. The condensate obtained in a cold trap has components of a complex, strongly acidic reaction system. Quantitative measurements to determine the composition and qualitative measurements to elucidate the structure are carried out using NMR. Complementary to this, analysis is carried out in the gas phase using gas chromatography.

Figure: Reactor for cold plasma.

Characterization of Heterogenous Catalysts

Solid-state NMR enables the characterization of solid materials at the atomic level. Magic Angle Spinning (MAS) is used to reduce the broadening of NMR signals due to anisotropic interactions, such as dipolar couplings, and to improve the resolution and sensitivity of the spectra. This technique finds application in the imaging and characterization of novel Janus particle catalysts with subsequent application in multiphase catalytic reactions.

Figure: Solid-state NMR spectrum and scanning electron micrograph of silica-based Janus particles.