Friday, March 4, 2016

Solid-State Dynamic Nuclear Polarization at 9.4 and 18.8 T from 100 K to Room Temperature

This is an incredible article. It shows the temperature dependence of the DNP enhancement over a wide temperature regime. Most importantly it shows that at room temperature still an enhancement of 15-20 can be achieved.
Just a few years ago the common believe was that solid-state MAS-DNP experiments have to be performed at 90 K or below. This article clearly demonstrates that there is still so much room for improvements of DNP. I think the most exciting moments in DNP are still ahead of us and the method has the potential to become an integral part of the DNP toolbox.



Lelli, M., et al., Solid-State Dynamic Nuclear Polarization at 9.4 and 18.8 T from 100 K to Room Temperature. J Am Chem Soc, 2015. 137(46): p. 14558-61.


Efficient dynamic nuclear polarization (DNP) in solids, which enables very high sensitivity NMR experiments, is currently limited to temperatures of around 100 K and below. Here we show how by choosing an adequate solvent, (1)H cross effect DNP enhancements of over 80 can be obtained at 240 K. To achieve this we use the biradical TEKPol dissolved in a glassy phase of ortho-terphenyl (OTP). We study the solvent DNP enhancement of both TEKPol and BDPA in OTP in the range from 100 to 300 K at 9.4 and 18.8 T. Surprisingly, we find that the DNP enhancement decreases only relatively slowly for temperatures below the glass transition of OTP (Tg = 243 K), and (1)H enhancements around 15-20 at ambient temperature can be observed. We use this to monitor molecular dynamic transitions in the pharmaceutically relevant solids Ambroxol and Ibuprofen.