title: High-resolution NMR of hydrogen in organic solids by DNP enhanced natural abundance deuterium spectroscopy.
abstract: We demonstrate that high field (9.4 T) dynamic nuclear polarization (DNP) at cryogenic (∼100 K) sample temperatures enables the rapid acquisition of natural abundance (1)H-(2)H cross-polarization magic angle spinning (CPMAS) solid-state NMR spectra of organic solids. Spectra were obtained by impregnating substrates with a solution of the stable DNP polarizing agent TEKPol in tetrachloroethane. Tetrachloroethane is a non-solvent for the solids, and the unmodified substrates are then polarized through spin diffusion. High quality natural abundance (2)H CPMAS spectra of histidine hydrochloride monohydrate, glycylglycine and theophylline were acquired in less than 2h, providing direct access to hydrogen chemical shifts and quadrupolar couplings. The spectral resolution of the (2)H solid-state NMR spectra is comparable to that of (1)H spectra obtained with state of the art homonuclear decoupling techniques.
authors.affiliation: Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland; Institut des Sciences Analytiques, Centre de RMN à très hauts champs (CNRS/ENS-Lyon, UCB-Lyon1), Université de Lyon, 69100 Villeurbanne, France.
authors.forename: Aaron J
authors.initials: AJ
authors.lastname: Rossini
authors.affiliation: Institut des Sciences Analytiques, Centre de RMN à très hauts champs (CNRS/ENS-Lyon, UCB-Lyon1), Université de Lyon, 69100 Villeurbanne, France.
authors.forename: Judith
authors.initials: J
authors.lastname: Schlagnitweit
authors.affiliation: Institut des Sciences Analytiques, Centre de RMN à très hauts champs (CNRS/ENS-Lyon, UCB-Lyon1), Université de Lyon, 69100 Villeurbanne, France.
authors.forename: Anne
authors.initials: A
authors.lastname: Lesage
authors.affiliation: Institut des Sciences et Ingénierie Chimiques, Ecole Polytechnique Fédérale de Lausanne (EPFL), CH-1015 Lausanne, Switzerland; Institut des Sciences Analytiques, Centre de RMN à très hauts champs (CNRS/ENS-Lyon, UCB-Lyon1), Université de Lyon, 69100 Villeurbanne, France. Electronic address: lyndon.emsley@epfl.ch.
authors.forename: Lyndon
authors.initials: L
authors.lastname: Emsley
mesh_terms: D003903:Deuterium / Q000032:analysis*; D004574:Electromagnetic Fields; D004980:Ethane / Q000031:analogs & derivatives / Q000737:chemistry; D006033:Glycylglycine / Q000737:chemistry; D006639:Histidine / Q000737:chemistry; D006843:Hydrocarbons, Chlorinated / Q000737:chemistry; D006859:Hydrogen / Q000737:chemistry; D007202:Indicators and Reagents; D009682:Magnetic Resonance Spectroscopy / Q000379:methods*; D013696:Temperature; D013806:Theophylline / Q000737:chemistry
chemical_list: D006843:Hydrocarbons, Chlorinated; D007202:Indicators and Reagents; D006033:Glycylglycine; C016134:tetrachloroethane; D006639:Histidine; D006859:Hydrogen; D003903:Deuterium; D013806:Theophylline; D004980:Ethane
keywords: Deuterium; Hyper-polarization; NMR spectroscopy