甲 (trimethylsilyl) 作为快速旋转固态NMR实验的标准化合物
Ruixian Han1, Alexander L Paterson2, Moses H Milchberg3
1Department of Chemistry, University of Wisconsin-Madison, Madison, WI, United States.
泰特拉基斯三甲基基 (TTMSS) 简化了超快速魔法角度旋转固态NMR的设置. 这种高信号对噪声的标准提供了精确的校准和引用,甚至与生物样本.
科学领域:
- 固态核磁共振 (SSNMR) 光谱学 固态核磁共振 (SSNMR) 光谱学
- 先进的光谱技术 技术
- 材料科学 材料科学 材料科学
背景情况:
- 超快速魔法角度旋转 (MAS) >100 kHz可以增强SSNMR的H检测.
- 对于高MAS速率的小型旋转器限制了样本体积和C敏感度.
- 传统的SSNMR标准对于超快的MAS,高场和可重现性是不够的.
研究的目的:
- 开发一个高信号噪声比 (SNR) 1H检测标准,用于超快的MAS SSNMR.
- 简化仪器设置,魔术角度校准和化学转移引用.
- 评估四甲三甲) (TTMSS) 作为一个多用途的标准.
主要方法:
- 使用TTMSS (TKS) 在~40kHz的MAS设置魔术角度和闪.
- 与传统的KBr和阿达曼坦标准进行比较.
- 使用四组分混合物 (TKS,阿达曼坦,标记为N-乙瓦林,KBr) 进行全面的探头校准.
主要成果:
- TTMSS (TKS) 实现了精确的魔术角度设置和闪.
- 与传统标准相比,在较短的时间内获得了有利的结果.
- 高SNR和类似TMS的TKS化学转移证明了它的实用性.
结论:
- TTMSS (TKS) 是一个高磁场超快速MAS SSNMR的有效标准.
- TKS简化了仪器配置和校准,提高了精度和效率.
- 在SSNMR中,TKS显示出作为生物样本的内部标准的潜力.
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