DNP-NMR · Easy DNP Enhanced Solid-State NMR: High Sample Temperatures and Low Microwave Powers
Horizon 2020 — Marie Skłodowska-Curie Actions
- Duration
- 2021-04-01 → 2023-03-31
- EU contribution
- €203,149
- Participants
- 1
- Scheme
- MSCA-IF
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Results in brief
Easy DNP Enhanced Solid-State NMR: High Sample Temperatures and Low Microwave Powers
Nuclear magnetic resonance (NMR) spectroscopy is an indispensable tool in chemical science to study atomic-level structures and dynamics, which is at the heart of rational design of materials for targeted applications. A number of critical research areas that impact society rely on structural characterization techniques like NMR spectroscopy, such as the development of materials for carbon-capture and sustainable energy (e.g. photovoltaics, batteries, catalysts, thermoelectrics etc.), pharmaceuticals research that involves urgent, new chemical modalities for drugs and vaccines, and biochemistry where the function of large biomolecules is linked to their atomic structures. However, NMR suffers from an intrinsically low sensitivity, resulting in long experiment times on the order of days for advanced experiments, prohibiting more complex experiments and high throughput. Dynamic nuclear polarization (DNP) is a promising approach to address this problem as it provides large gains in signal-to-noise ratio by a factor of 100-200 in NMR spectra. The sensitivity gains provided by DNP have enabled critical questions to be answered in several research areas. However, DNP currently requires cryogenic temperatures (−170 °C) and expensive specialized equipment, with only around 55 DNP instruments worldwide at present. To enable widespread adoption of DNP, it is critical to develop this technology further and extend the range of possible samples and temperatures. The primary bottleneck for improved DNP is the efficacy of the polarizing agents that are added to the sample to provide the greater sensitivity. The objective of this project was to develop robust DNP polarizing agents and DNP methods at higher temperatures (–70 to 30 °C), that will allow DNP-enhanced NMR to become the tool of choice for chemists, material scientists and biologists.
Data: CORDIS, © European Union
Project objective
NMR (nuclear magnetic resonance) spectroscopy is limited by low sensitivity. Recently, it has been shown that a technique called DNP (dynamic nuclear polarization) can enhance solid-state NMR signals by orders of magnitude. DNP has enabled the determination of atomic-level structure in solids by accelerating complex multidimensional NMR experiments. However, only expert NMR spectroscopists apply DNP. This is because, DNP solid-state NMR requires highly specialized, large and expensive, dedicated equipment. Currently, DNP experiments are performed with high power microwave sources (gyrotrons) and low sample temperatures near 100 K. Gyrotrons and low-temperature control systems place a large demand on the building infrastructure and require expertise for routine operation. Additionally, a low sample temperature reduces the resolution of NMR spectra dramatically, which hinders the characterization of chemical structure.This project aims to develop methods that will simplify the application of DNP and enable its widespread utilization. We will develop methodology to perform DNP at high sample temperatures and low microwave powers, using compact microwave sources such as klystrons. Specifically, we will focus on the development of polarizing agents designed for low power and sample formulations that are optimized for high temperatures. Finally, we will perform liquid state Overhauser DNP at high temperatures and transfer the polarization to the surface of materials. The proposed advances will eliminate the need for a gyrotron and low-temperature equipment and therefore, will simplify the DNP experimental setup. This will enable the broad application of DNP to solve challenging problems in chemistry, materials science and biology that are inaccessible using conventional solid-state NMR.
Original text from CORDIS.
Participants
- ECOLE POLYTECHNIQUE FEDERALE DE LAUSANNE · LausanneCoordinatorSwitzerland
Links
Data: CORDIS, © European Union