Sensitivity enhancement via multiple contacts in the {1H-29Si}-1H cross polarization experiment: a case study of modified silica nanoparticle surfaces

通过 {1H-29Si}-1H 交叉极化实验中的多重接触提高灵敏度:改性二氧化硅纳米粒子表面的案例研究

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作者:Chuanyu Yan, François Kayser, Reiner Dieden

Abstract

{1H-29Si}-1H double cross polarization inverse detection (DCPi) solid-state NMR, has recently been shown to be a powerful tool for studying molecules adsorbed on the silica surface. In this contribution, we develop an improved version (MCPi) which incorporates a block of multiple contact pulses, and quantitatively compare the sensitivities of MCPi and DCPi over a typical range of experimental parameters. The MCPi pulse sequence aims at higher sensitivity and robustness for studying samples with various relaxation characteristics. In the case of dimethyl sulfoxide (DMSO) molecules adsorbed on the silica surface, MCPi performs equally well or up to 2.5 times better than DCPi over a wide range of parameters. The applicability to and performance of MCPi on composite materials was demonstrated using a sample of polymer-silica composite, where significantly higher sensitivity could be achieved at very long total mixing times. The results also showed that both techniques are surface specific in the sense that only the groups close to the surface can be detected.

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