Björgvinsdóttir, Snædís, Brennan J. Walder, Nicolas Matthey, and Lyndon Emsley. “Maximizing Nuclear Hyperpolarization in Pulse Cooling under MAS.” Journal of Magnetic Resonance 300 (March 2019): 142–48.
https://doi.org/10.1016/j.jmr.2019.01.011.
It has recently been shown how dynamic nuclear polarization can be used to hyperpolarize the bulk of proton-free solids. This is achieved by generating the polarization in a wetting phase, transferring it to nuclei near the surface and relaying it towards the bulk through homonuclear spin diffusion between weakly magnetic nuclei. Pulse cooling is a strategy to achieve this that uses a multiple contact cross-polarization sequence for bulk hyperpolarization. Here, we show how to maximize sensitivity using the pulse cooling method by experimentally optimizing pulse parameters and delays on a sample of powdered SnO2. To maximize sensitivity we introduce an approach where the magic angle spinning rate is modulated during the experiment: the CP contacts are carried out at a slow spin rate to benefit from faster spin diffusion, and the spin rate is then accelerated before detection to improve line narrowing. This method can improve the sensitivity of pulse cooling for 119Sn spectra of SnO2 by an additional factor of 3.5.