Wang Qiang, Trébosc Julien, Li Yixuan, Lafon Oliver, Xin Shaohui, Xu Jun, Hu Bingwen, Feng Ningdong, Amoureux Jean-Paul, Deng Feng
National Center for Magnetic Resonance in Wuhan, State Key Laboratory of Magnetic Resonance and Atomic and Molecular Physics, Wuhan Institute of Physics and Mathematics, Chinese Academy of Sciences, 430071 Wuhan, China.
Univ. Lille, CNRS-8181, ENSCL, UCCS-Unit of Catalysis and Chemistry of Solids, 59000 Lille, France.
J Magn Reson. 2018 Aug;293:92-103. doi: 10.1016/j.jmr.2018.06.005. Epub 2018 Jun 15.
We introduce two MAS schemes that allow manipulating the satellite-transition (ST) populations of half-integer quadrupolar nuclei, and which both exhibit improved robustness to the quadrupolar coupling constant (C). These schemes, called quadruple frequency sweep (QFS) or quadruple WURST (QWURST) are the sums of two DFS or four WURST to efficiently invert the ST populations of nuclei subject to large or small quadrupole interactions, simultaneously. These quadruple sweeps methods only require 6% more rf-power than the double sweeps ones. We demonstrate, both numerically and experimentally, that the QFS and QWURST schemes benefit from robustness to C and rf amplitude and offset and hence achieve uniform enhancement of the CT signal for Al nuclei subject to different quadrupole interactions. Although the version of QFS with repetitive accumulation can achieve higher enhancement in the S/N of the Al MAS spectrum, the final sensitivity gains mainly depend on the longitudinal relaxation time of different Al sites. We also confirm that these schemes provide an improved acceleration of the P-{Al} coherence transfer in PT-J-HMQC experiments.
我们介绍了两种可以操纵半整数四极核卫星跃迁(ST)布居数的MAS方案,这两种方案对四极耦合常数(C)均具有更高的稳健性。这些方案被称为四频扫频(QFS)或四脉冲WURST(QWURST),它们分别是两个DFS或四个WURST的总和,能够同时有效地反转受大或小四极相互作用影响的核的ST布居数。这些四频扫频方法所需的射频功率仅比双频扫频方法多6%。我们通过数值模拟和实验证明,QFS和QWURST方案得益于对C以及射频幅度和偏移的稳健性,因此对于受不同四极相互作用影响的Al核,能够实现CT信号的均匀增强。尽管具有重复累加的QFS版本可以在Al MAS谱的信噪比方面实现更高的增强,但最终的灵敏度增益主要取决于不同Al位点的纵向弛豫时间。我们还证实,这些方案在PT-J-HMQC实验中能够加快P-{Al}相干转移。