Instrumentation for cryogenic magic angle spinning dynamic nuclear polarization using 90L of liquid nitrogen per day

• Published in: Journal of magnetic resonance (1997) 2017-10, Vol.283, p.71-78
• Main Authors: Albert, Brice J., Pahng, Seong Ho, Alaniva, Nicholas, Sesti, Erika L., Rand, Peter W., Saliba, Edward P., Scott, Faith J., Choi, Eric J., Barnes, Alexander B.
• Format: Article
• Language: English
• Subjects: Cold Temperature; Cryogenic MAS; Dynamic nuclear polarization; Electron decoupling; Gases; Heat exchanger; Magic-angle spinning; Magnetic Resonance Spectroscopy - instrumentation; Magnetic Resonance Spectroscopy - methods; Microwaves; Nitrogen - chemistry; Pulsed DNP; Solid-state NMR; Temperature; Urea - chemistry
• ISSN: 1090-7807; 1096-0856
• DOI: 10.1016/j.jmr.2017.08.014

[Display omitted] •Counterflow heat exchanger design reduces nitrogen consumption to 90L/day.•Computational fluid dynamics analysis describes heat exchanger performance.•80K sample temperature yields DNP enhancement of 328.•Robust design and low H2O content permits extended continuous operation (>5weeks). Cryogenic sample temperatures can enhance NMR sensitivity by extending spin relaxation times to improve dynamic nuclear polarization (DNP) and by increasing Boltzmann spin polarization. We have developed an efficient heat exchanger with a liquid nitrogen consumption rate of only 90L per day to perform magic-angle spinning (MAS) DNP experiments below 85K. In this heat exchanger implementation, cold exhaust gas from the NMR probe is returned to the outer portion of a counterflow coil within an intermediate cooling stage to improve cooling efficiency of the spinning and variable temperature gases. The heat exchange within the counterflow coil is calculated with computational fluid dynamics to optimize the heat transfer. Experimental results using the novel counterflow heat exchanger demonstrate MAS DNP signal enhancements of 328±3 at 81±2K, and 276±4 at 105±2K.