A dedicated spectrometer for dissolution DNP NMR spectroscopy

被引:84
|
作者
Leggett, James [1 ]
Hunter, Robert [2 ]
Granwehr, Josef [1 ]
Panek, Rafal [1 ]
Perez-Linde, Angel J. [1 ]
Horsewill, Anthony J.
McMaster, Jonathan [3 ]
Smith, Graham [2 ]
Koeckenberger, Walter [1 ]
机构
[1] Univ Nottingham, Sch Phys & Astron, Sir Peter Mansfield Magnet Resonance Ctr, Nottingham NG7 2RD, England
[2] Univ St Andrews, Sch Phys & Astron, St Andrews KY16 9SS, Fife, Scotland
[3] Univ Nottingham, Sch Chem, Nottingham NG7 2RD, England
基金
英国工程与自然科学研究理事会;
关键词
NUCLEAR; PERFORMANCE; DESIGN; FIELD; SENSITIVITY; WAVE;
D O I
10.1039/c002566f
中图分类号
O64 [物理化学(理论化学)、化学物理学];
学科分类号
070304 ; 081704 ;
摘要
Using low temperature dynamic nuclear polarisation (DNP) in conjunction with dissolution makes it possible to generate highly polarised nuclear spin systems for liquid state applications of nuclear magnetic resonance spectroscopy. However, in its current implementation, which requires the transfer of the solute between two different magnets, the hyperpolarisation strategy is limited to spin systems with relatively long longitudinal relaxation time constants. Here we describe the design and construction of a dedicated spectrometer for DNP applications that is based on a magnet with two isocentres. DNP enhancement is carried out in the upper compartment of this magnet in a low temperature environment at 3.35 T, while a 9.4 T isocentre in the lower compartment is used for high resolution NMR spectroscopy. The close proximity (85 cm) of the two isocentres makes it possible to transfer the sample in the solid state with very little loss of spin polarisation. In first performance tests this novel experimental set-up proved to be superior to the strategy involving two separate magnets.
引用
收藏
页码:5883 / 5892
页数:10
相关论文
共 50 条
  • [1] Compact, low-cost NMR spectrometer and probe for dissolution DNP
    Albannay, Mohammed M.
    Vinther, Joachim M. O.
    Petersen, Jan Raagaard
    Zhurbenko, Vitaliy
    Ardenkjaer-Larsen, Jan Henrik
    JOURNAL OF MAGNETIC RESONANCE, 2019, 304 : 7 - 15
  • [2] Dissolution DNP-NMR spectroscopy using galvinoxyl as a polarizing agent
    Lumata, Lloyd L.
    Merritt, Matthew E.
    Malloy, Craig R.
    Sherry, A. Dean
    van Tol, Johan
    Song, Likai
    Kovacs, Zoltan
    JOURNAL OF MAGNETIC RESONANCE, 2013, 227 : 14 - 19
  • [3] Applications of Dissolution-DNP for NMR Screening
    Kim, Yaewon
    Hilty, Christian
    BIOLOGICAL NMR, PT B, 2019, 615 : 501 - 526
  • [4] Cryogenic and Dissolution DNP NMR on γ-Irradiated Organic Molecules
    Giannoulis, Angeliki
    Butbul, Korin
    Carmieli, Raanan
    Kim, Jihyun
    Montrazi, Elton Tadeu
    Singh, Kawarpal
    Frydman, Lucio
    JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2024, 146 (30) : 20758 - 20769
  • [5] Chiral Recognition by Dissolution DNP NMR Spectroscopy of 13C-Labeled DL-Methionine
    Monteagudo, Eva
    Virgili, Albert
    Parella, Teodor
    Perez-Trujillo, Miriam
    ANALYTICAL CHEMISTRY, 2017, 89 (09) : 4939 - 4944
  • [6] A SPECTROMETER FOR EPR, DNP, AND MULTINUCLEAR HIGH-RESOLUTION NMR
    SINGEL, DJ
    SEIDEL, H
    KENDRICK, RD
    YANNONI, CS
    JOURNAL OF MAGNETIC RESONANCE, 1989, 81 (01): : 145 - 161
  • [7] The gyrotron for DNP-NMR spectroscopy: A review
    Nowak, Kacper
    BULLETIN OF THE POLISH ACADEMY OF SCIENCES-TECHNICAL SCIENCES, 2022, 70 (01)
  • [8] High-field NMR with dissolution triplet-DNP
    Kagawa, Akinori
    Miyanishi, Koichiro
    Ichijo, Naoki
    Negoro, Makoto
    Nakamura, Yushi
    Enozawa, Hideo
    Murata, Tsuyoshi
    Morita, Yasushi
    Kitagawa, Masahiro
    JOURNAL OF MAGNETIC RESONANCE, 2019, 309
  • [9] Real-Time Analysis of Folding upon Binding of a Disordered Protein by Using Dissolution DNP NMR Spectroscopy
    Ragavan, Mukundan
    Iconaru, Luigi I.
    Park, Cheon-Gil
    Kriwacki, Richard W.
    Hilty, Christian
    ANGEWANDTE CHEMIE-INTERNATIONAL EDITION, 2017, 56 (25) : 7070 - 7073
  • [10] Multi-Barrel Gyrotron for DNP/NMR Spectroscopy
    Zapevalov, V. E.
    Zuev, A. S.
    Plankin, O. P.
    RADIOPHYSICS AND QUANTUM ELECTRONICS, 2023, 66 (01) : 1 - 18