title: Low-temperature dynamic nuclear polarization with helium-cooled samples and nitrogen-driven magic-angle spinning.
abstract: We describe novel instrumentation for low-temperature solid state nuclear magnetic resonance (NMR) with dynamic nuclear polarization (DNP) and magic-angle spinning (MAS), focusing on aspects of this instrumentation that have not been described in detail in previous publications. We characterize the performance of an extended interaction oscillator (EIO) microwave source, operating near 264 GHz with 1.5 W output power, which we use in conjunction with a quasi-optical microwave polarizing system and a MAS NMR probe that employs liquid helium for sample cooling and nitrogen gas for sample spinning. Enhancement factors for cross-polarized (13)C NMR signals in the 100-200 range are demonstrated with DNP at 25K. The dependences of signal amplitudes on sample temperature, as well as microwave power, polarization, and frequency, are presented. We show that sample temperatures below 30K can be achieved with helium consumption rates below 1.3 l/h. To illustrate potential applications of this instrumentation in structural studies of biochemical systems, we compare results from low-temperature DNP experiments on a calmodulin-binding peptide in its free and bound states.
authors.affiliation: Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases, National Institutes of Health, Bethesda, MD 20892-0520, United States.
authors.forename: Kent
authors.initials: K
authors.lastname: Thurber
authors.affiliation: Laboratory of Chemical Physics, National Institute of Diabetes and Digestive and Kidney Diseases, National Institutes of Health, Bethesda, MD 20892-0520, United States. Electronic address: robertty@mail.nih.gov.
authors.forename: Robert
authors.initials: R
authors.lastname: Tycko
mesh_terms: D003080:Cold Temperature; D006371:Helium / Q000737:chemistry*; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D008872:Microwaves; D009584:Nitrogen / Q000737:chemistry*
chemical_list: D006371:Helium; D009584:Nitrogen
keywords: Dynamic nuclear polarization; Low-temperature NMR; Magic-angle spinning; Protein structure; Solid state NMR