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.)
Improved sensitivity and quantification for 29Si NMR experiments on solids using UDEFT (Uniform Driven Equilibrium Fourier Transform).
Solid State Nuclear Magnetic Resonance ( IF 3.2 ) Pub Date : 2019-03-26 , DOI: 10.1016/j.ssnmr.2019.03.007
Nghia Tuan Duong 1 , Julien Trébosc 2 , Olivier Lafon 3 , Jean-Paul Amoureux 4
Affiliation  

We demonstrate the possibility to use UDEFT (Uniform Driven Equilibrium Fourier Transform) technique in order to improve the sensitivity and the quantification of one-dimensional 29Si NMR experiments under magic-angle spinning (MAS). We derive an analytical expression of the signal-to-noise ratios of UDEFT and single-pulse (SP) experiments subsuming the contributions of transient and steady-state regimes. Using numerical spin dynamics simulations and experiments on 29Si-enriched amorphous silica and borosilicate glass, we show that 59180298059180 refocusing composite π-pulse and the adiabatic inversion using tanh/tan modulation improve the robustness of UDEFT technique to rf-inhomogeneity, offset, and chemical shift anisotropy. These pulses combined with a two-step phase cycle limit the pulse imperfections and the artifacts produced by stimulated echoes. The sensitivity of SP, UDEFT and CPMG (Carr-Purcell-Meiboom-Gill) techniques are experimentally compared on functionalized and non-functionalized mesoporous silica. Furthermore, experiments on a flame retardant material prove that UDEFT technique provides a better quantification of 29Si sites with higher sensitivity than SP method.



中文翻译:

使用UDEFT(均匀驱动平衡傅立叶变换)对固体进行29Si NMR实验的改进的灵敏度和定量。

我们证明了使用UDEFT(均匀驱动平衡傅立叶变换)技术的可能性,以提高灵敏角旋转(MAS)下一维29 Si NMR实验的灵敏度和定量。我们推导了UDEFT和单脉冲(SP)实验的信噪比的分析表达式,其中包含了瞬态和稳态机制的贡献。使用数值自旋动力学模拟和29种富硅非晶硅和硼硅酸盐玻璃的实验,我们得出59 180 298 0 59 180复合π脉冲的重新聚焦以及使用tanh / tan调制的绝热反演提高了UDEFT技术对rf不均匀性,偏移和化学位移各向异性的鲁棒性。这些脉冲与两步相位周期相结合,限制了脉冲缺陷和受激回波产生的伪像。SP,UDEFT和CPMG(Carr-Purcell-Meiboom-Gill)技术的灵敏度在功能化和非功能化介孔二氧化硅上进行了实验比较。此外,在阻燃材料上进行的实验证明,与SP方法相比,UDEFT技术可以更好地量化29个Si位,灵敏度更高。

更新日期:2019-03-26
down
wechat
bug