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用于在13C NMR中进行非常精确的强度测量的绝热1H去耦方案。

Adiabatic 1H decoupling scheme for very accurate intensity measurements in 13C NMR.

作者信息

Tenailleau Eve, Akoka Serge

机构信息

LAIEM-CNRS UMR 6006, Faculté des Sciences et Techniques-Université de NANTES, 2 rue de la Houssinière-BP 92208, 44322 NANTES cedex 3, France.

出版信息

J Magn Reson. 2007 Mar;185(1):50-8. doi: 10.1016/j.jmr.2006.11.007. Epub 2006 Dec 4.

Abstract

Adiabatic proton decoupling has been optimized in order to obtain accurate quantitative measurements of intensities on 13C NMR spectra. For each offset, the minimum adiabaticity factor (Km) reached during the pulse was computed. This K(m) profile was used to optimize the peak value and the swept frequency range of the adiabatic pulses. With a cosinus amplitude modulation, offset-independent-adiabaticity, and the M4P5-M4P9-M4P5'-M4P9' phase cycle, an accuracy of 2 per thousand for the 13C NMR measurements was reached. An approach using bi-labeled 13C acetic acid and ethanol at 99% allowed a fine experimental determination of the uniformity of the decoupling profile. The comparison with WALTZ-16 highlights the improvements in the uniformity of the proton decoupling.

摘要

为了在13C NMR谱上获得准确的强度定量测量结果,对绝热质子去耦进行了优化。对于每个偏移量,计算脉冲期间达到的最小绝热因子(Km)。该K(m) 曲线用于优化绝热脉冲的峰值和扫频范围。通过余弦幅度调制、与偏移无关的绝热性以及M4P5-M4P9-M4P5'-M4P9' 相位循环,13C NMR测量的精度达到了千分之二。使用99% 的双标记13C乙酸和乙醇的方法可以对去耦曲线的均匀性进行精细的实验测定。与WALTZ-16的比较突出了质子去耦均匀性的改进。

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