当前位置: X-MOL 学术Solid State Nucl. Magn. Reson. › 论文详情
Our official English website, www.x-mol.net, welcomes your feedback! (Note: you will need to create a separate account there.)
Combining fast magic angle spinning dynamic nuclear polarization with indirect detection to further enhance the sensitivity of solid-state NMR spectroscopy.
Solid State Nuclear Magnetic Resonance ( IF 3.2 ) Pub Date : 2020-08-11 , DOI: 10.1016/j.ssnmr.2020.101685
Zhuoran Wang 1 , Michael P Hanrahan 1 , Takeshi Kobayashi 2 , Frédéric A Perras 2 , Yunhua Chen 1 , Frank Engelke 3 , Christian Reiter 3 , Armin Purea 3 , Aaron J Rossini 1 , Marek Pruski 1
Affiliation  

Dynamic nuclear polarization (DNP) and indirect detection are two commonly applied approaches for enhancing the sensitivity of solid-state NMR spectroscopy. However, their use in tandem has not yet been investigated. With the advent of low-temperature fast magic angle spinning (MAS) probes with 1.3-mm diameter rotors capable of MAS at 40 ​kHz it becomes feasible to combine these two techniques. In this study, we performed DNP-enhanced 2D indirectly detected heteronuclear correlation (idHETCOR) experiments on 13C, 15N, 113Cd and 89Y nuclei in functionalized mesoporous silica, CdS nanoparticles, and Y2O3 nanoparticles. The sensitivity of the 2D idHETCOR experiments was compared with those of DNP-enhanced directly-detected 1D cross polarization (CP) and 2D HETCOR experiments performed with a standard 3.2-mm rotor. Due to low CP polarization transfer efficiencies and large proton linewidth, the sensitivity gains achieved by indirect detection alone were lower than in conventional (non-DNP) experiments. Nevertheless, despite the smaller sample volume the 2D idHETCOR experiments showed better absolute sensitivities than 2D HETCOR experiments for nuclei with the lowest gyromagnetic ratios. For 89Y, 2D idHETCOR provided 8.2 times better sensitivity than the 1 D89Y-detected CP experiment performed with a 3.2-mm rotor.



中文翻译:

将快速幻角旋转动态核极化与间接检测相结合,可以进一步提高固态NMR光谱的灵敏度。

动态核极化(DNP)和间接检测是提高固态NMR光谱灵敏度的两种常用方法。但是,尚未研究它们的串联使用。随着低温快速魔术角旋转(MAS)探头的出现,直径为1.3 mm的转子能够在40 kHz下进行MAS,将这两种技术结合起来变得可行。在这项研究中,我们对功能化介孔二氧化硅,CdS纳米颗粒和Y 2 O 3中的13 C,15 N,113 Cd和89 Y核进行了DNP增强的2D间接检测异核相关性(idHETCOR)实验。纳米粒子。将2D idHETCOR实验的灵敏度与DNP增强的直接检测的1D交叉极化(CP)和使用标准3.2 mm转子进行的2D HETCOR实验的灵敏度进行了比较。由于CP极化转移效率低和质子线宽大,仅通过间接检测获得的灵敏度增益就低于常规(非DNP)实验。尽管如此,尽管样品体积较小,但对于具有最低旋磁比的原子核,2D idHETCOR实验显示的绝对灵敏度要高于2D HETCOR实验。对于89 Y,二维IDHETCOR的灵敏度是对3.2 mm转子进行的1 D 89 Y检测的CP实验的8.2倍。

更新日期:2020-09-13
down
wechat
bug