Bruker Japan K.K., 3-9, Moriya-cho, Kanagawa-ku, Yokohama-shi, Kanagawa 221-0022, Japan.
Univ. Lille, CNRS, Centrale Lille, ENSCL, Univ. Artois, UMR 8181 - UCCS - Unit of Catalysis and Chemistry of Solids, F-59000 Lille, France.
J Magn Reson. 2021 Aug;329:107028. doi: 10.1016/j.jmr.2021.107028. Epub 2021 Jun 25.
In this article, we compare the various schemes of magnetization transfer from half-integer quadrupolar spins to H nuclei and we establish an efficient protocol to perform these transfers under MQMAS high-resolution with the MQ-HETCOR and MQ-SPAM-HETCOR experiments under fast MAS. The MQMAS efficiencies are analyzed with SIMPSON simulations, and the CPMAS and RINEPT magnetization transfers are compared at 62.5 kHz MAS using {Na}-H and {Al}-H MQ-HETCOR and MQ-SPAM-HETCOR experiments performed on NaHPO4, NaHPO, Na citrate dihydrate and ipa-AlPO-14 powder samples. We discuss the pros and cons of these approaches, aiming to record 2D spectra of the best possible quality under fast MAS. We also incorporate some experimental approaches to reduce the total experiment time of such long 2D experiments.
在本文中，我们比较了从半整数 quadrupolar 自旋到 H 核的各种磁化转移方案，并建立了一种有效的方案，以便在快速 MAS 下通过 MQMAS 高分辨率实验（MQ-HETCOR 和 MQ-SPAM-HETCOR 实验）执行这些转移。使用 SIMPSON 模拟分析了 MQMAS 的效率，并在 62.5 kHz MAS 下比较了 CPMAS 和 RINEPT 磁化转移，方法是在 NaHPO4、NaHPO 和 Na 柠檬酸盐二水合物以及 ipa-AlPO-14 粉末样品上进行 {Na}-H 和 {Al}-H MQ-HETCOR 和 MQ-SPAM-HETCOR 实验。我们讨论了这些方法的优缺点，旨在在快速 MAS 下记录尽可能高质量的 2D 谱。我们还结合了一些实验方法来减少这种长 2D 实验的总实验时间。
