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Dendritic polarizing agents for DNP SENS.

Wei-Chih Liao1, Ta-Chung Ong1, David Gajan2

  • 1Department of Chemistry and Applied Biosciences , ETH Zürich , Vladimir-Prelog-Weg 1-5 , 8093 Zürich , Switzerland .

Chemical Science
|April 29, 2017
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Summary

We developed novel carbosilane dendrimers for Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy (DNP SENS). These agents minimize radical interactions, preserving surface signals and enhancing studies of reactive catalysts.

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Area of Science:

  • Solid-state NMR Spectroscopy
  • Surface Chemistry
  • Materials Science

Background:

  • Dynamic Nuclear Polarization Surface Enhanced NMR Spectroscopy (DNP SENS) significantly enhances solid-state NMR for surface analysis.
  • Conventional DNP polarizing agents can cause undesirable nuclear spin relaxation and react with substrates, especially problematic for heterogeneous catalysts.
  • Reducing direct interaction between polarizing agents and surfaces is key to overcoming these limitations.

Purpose of the Study:

  • To develop novel polarizing agents for DNP SENS that mitigate drawbacks of traditional agents.
  • To investigate carbosilane-based dendritic structures as potential polarizing agents.
  • To demonstrate the preservation of surface nuclear spin properties and enhancement of reactive catalyst studies.

Main Methods:

  • Synthesis of carbosilane-based dendritic polarizing agents.
  • Application of these agents in DNP SENS experiments.
  • Evaluation of nuclear spin relaxation times (T'2) of surface species.
  • Testing the agents on a reactive heterogeneous metathesis catalyst.

Main Results:

  • The bulky dendrimer structure effectively shields the solid surface from the free radical.
  • Long nuclear T'2 relaxation times of surface species were preserved.
  • Successful signal enhancement was achieved for a reactive heterogeneous metathesis catalyst.

Conclusions:

  • Carbosilane-based dendritic polarizing agents offer a solution to overcome limitations of conventional DNP SENS agents.
  • These novel agents enable high-resolution solid-state NMR investigations of sensitive or reactive surfaces.
  • The approach is promising for studying complex heterogeneous catalytic systems.