Satellite-Transition MAS: A New Technique for High-Resolution Quadrupolar NMR

卫星传输 MAS：高分辨率四极核磁共振新技术

• 批准号: GR/T23824/01
• 负责人: Stephen Wimperis
• 金额: $ 29.3万
• 依托单位: University of Glasgow
• 依托单位国家: 英国
• 项目类别: Research Grant
• 财政年份: 2006
• 资助国家: 英国
• 起止时间: 2006 至 无数据
• 项目状态: 已结题
• 来源: https://gtr.ukri.org/projects?ref=GR%2FT23824%2F01
• 关键词: Satellite; Transition; MAS; New; Technique

The recently developed multiple-quantum (MQ) magic-angle-spinning (MAS) and satellite-transition (ST) MAS experiments allow truly high-resolution NMR spectra of important quadrupolar nuclei, such as 17-0, 23-Na and 27-Al, to be obtained in solids using only conventional hardware. These new techniques are already being used extensively in both academia and industry to study minerals, glasses, zeolites and other microporous materials. We have been working on the development of these methods since 1995 and our research in this area has achieved wide international recognition. The two previous EPSRC grants that supported this work (GR/M12209 and GR/N07622) yielded over 25 publications and were rated extremely highly by assessors, but both have now expired.The aim of the the present proposal is to allow us to develop the STMAS method further. This is a particularly exciting new technique as it has much higher sensitivity than the older MAMAS method, while a number of interesting and unusual spin interactions are evidenced only in STMAS spectra. The technique is still very much in its infancy, since it appeared only during 2000, after the award of grant GRIN07622. In particular, we plan to improve the sensitivity of the technique still further and to develop the STMAS NMR experiment as a method of (a) recording high-resolution 25-Mg, 47-Ti and 95-Mo spectra without isotopic enrichment, and (b) studying the effects of second-order cross-term and third-order quadrupolar interactions on satellite transitions. We also aim to develop further our new SCAM (self-compensated for angle misset) variant of STMAS.

最近发展的多量子魔角自旋（MAS）和卫星跃迁（ST）MAS实验允许仅使用常规硬件在固体中获得重要四极核（如17-0、23-Na和27-Al）的真正高分辨率NMR谱。这些新技术已经在学术界和工业界广泛用于研究矿物、玻璃、沸石和其他微孔材料。自1995年以来，我们一直致力于开发这些方法，我们在这一领域的研究已获得广泛的国际认可。支持这项工作的前两个EPSRC赠款（GR/M12209和GR/N 07622）产生了超过25篇出版物，并得到了评估人员的高度评价，但现在都已过期。本提案的目的是让我们进一步发展STMAS方法。这是一项特别令人兴奋的新技术，因为它比旧的MAMAS方法具有更高的灵敏度，而许多有趣和不寻常的自旋相互作用仅在STMAS光谱中得到证明。这项技术仍然处于起步阶段，因为它只出现在2000年，在授予GRIN 07622之后。特别是，我们计划进一步提高该技术的灵敏度，并开发STMAS NMR实验作为一种方法，（a）记录高分辨率的25-Mg，47-Ti和95-Mo光谱没有同位素富集，（B）研究二阶交叉项和三阶四极相互作用对卫星跃迁的影响。我们还打算进一步开发STMAS的新SCAM（角度错位自补偿）变体。

项目成果

Satellite transitions acquired in real time by magic angle spinning (STARTMAS): "ultrafast" high-resolution MAS NMR spectroscopy of spin I=3/2 nuclei.

通过魔角旋转 (STARTMAS) 实时获取的卫星跃迁：自旋 I=3/2 原子核的“超快”高分辨率 MAS NMR 光谱。

• DOI: 10.1063/1.2813892
• 发表时间: 2008
• 期刊: The Journal of chemical physics
• 作者: Thrippleton MJ