Research output: Contribution to journal › Article › peer-review
Gas-Phase NMR of Hyperpolarized Propane with 1H-to-13C Polarization Transfer by PH-INEPT. / Burueva, Dudari B.; Kozinenko, Vitaly P.; Sviyazov, Sergey et al.
In: Applied Magnetic Resonance, Vol. 53, No. 3-5, 05.2022, p. 653-669.Research output: Contribution to journal › Article › peer-review
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TY - JOUR
T1 - Gas-Phase NMR of Hyperpolarized Propane with 1H-to-13C Polarization Transfer by PH-INEPT
AU - Burueva, Dudari B.
AU - Kozinenko, Vitaly P.
AU - Sviyazov, Sergey
AU - Kovtunova, Larisa M.
AU - Bukhtiyarov, Valerii
AU - Chekmenev, Eduard Y.
AU - Salnikov, Oleg G.
AU - Kovtunov, Kirill
AU - Koptyug, Igor
N1 - Funding Information: The HET-PHIP experiments performed by DBB, SVS, OGS, and IVK were funded by Russian Foundation for Basic Research (RFBR; Grants no. 19-29-10003 and 19-33-60045). The spin dynamics calculation performed by VPK was supported by RFBR grant no. 19-29-10028. The catalyst preparation performed by LMK was supported by the Ministry of Science and Higher Education of the Russian Federation (project # AAAA-A21-121011390011-4). EYC thanks the following for funding support: DOD CDMRP W81XWH15-1-0271 and W81XWH-20-10576, National Heart, Lung, and Blood Institute 1 R21 HL154032-01 and NSF CHE-1904780. Publisher Copyright: © 2021, The Author(s), under exclusive licence to Springer-Verlag GmbH Austria, part of Springer Nature.
PY - 2022/5
Y1 - 2022/5
N2 - In this work we demonstrate the possibility to transfer parahydrogen-derived 1H polarization to 13C nuclei in the gas phase using PH-INEPT-based pulse sequences. The propane with hyperpolarized 1H nuclei was produced via hydrogenation of propylene (at natural 13C abundance) with parahydrogen over the heterogeneous 1 wt% Rh/TiO2 catalyst at 7.05 T magnetic field of a NMR spectrometer. The apparent proton polarization was estimated as 1.8 ± 0.4%, taking into account the polarization losses caused by spin relaxation. The optimal inter-pulse delays for both the PH-INEPT and the PH-INEPT + sequences were determined via the numerical calculations considering the full spin system of propane which includes eight protons and one 13C nucleus. The application of the optimized PH-INEPT polarization transfer sequence resulted in the 13C polarization values of 0.07 ± 0.01% and 0.030 ± 0.006% for the methyl group of [1-13C]propane and the methylene group of [2-13C]propane, respectively. The experimental dependence of the 13C polarization values for [1-13C]propane and [2-13C]propane on the inter-pulse delay τ1 of the PH-INEPT sequence is in a good agreement with the simulation. The resulting 13C polarization using PH-INEPT + sequence is ~ 2.5 times lower than that via PH-INEPT, which is also consistent with the numerical calculations.
AB - In this work we demonstrate the possibility to transfer parahydrogen-derived 1H polarization to 13C nuclei in the gas phase using PH-INEPT-based pulse sequences. The propane with hyperpolarized 1H nuclei was produced via hydrogenation of propylene (at natural 13C abundance) with parahydrogen over the heterogeneous 1 wt% Rh/TiO2 catalyst at 7.05 T magnetic field of a NMR spectrometer. The apparent proton polarization was estimated as 1.8 ± 0.4%, taking into account the polarization losses caused by spin relaxation. The optimal inter-pulse delays for both the PH-INEPT and the PH-INEPT + sequences were determined via the numerical calculations considering the full spin system of propane which includes eight protons and one 13C nucleus. The application of the optimized PH-INEPT polarization transfer sequence resulted in the 13C polarization values of 0.07 ± 0.01% and 0.030 ± 0.006% for the methyl group of [1-13C]propane and the methylene group of [2-13C]propane, respectively. The experimental dependence of the 13C polarization values for [1-13C]propane and [2-13C]propane on the inter-pulse delay τ1 of the PH-INEPT sequence is in a good agreement with the simulation. The resulting 13C polarization using PH-INEPT + sequence is ~ 2.5 times lower than that via PH-INEPT, which is also consistent with the numerical calculations.
KW - PARAHYDROGEN-INDUCED POLARIZATION
KW - LIVED SPIN STATES
KW - PARA-HYDROGEN
KW - HETEROGENEOUS HYDROGENATION
KW - CATALYTIC-HYDROGENATION
KW - SIGNAL ENHANCEMENT
KW - ORDER TRANSFER
KW - C-13
KW - RELAXATION
KW - H-1
UR - http://www.scopus.com/inward/record.url?scp=85128383371&partnerID=8YFLogxK
U2 - 10.1007/s00723-021-01377-4
DO - 10.1007/s00723-021-01377-4
M3 - Article
VL - 53
SP - 653
EP - 669
JO - Applied Magnetic Resonance
JF - Applied Magnetic Resonance
SN - 0937-9347
IS - 3-5
ER -
ID: 34729559