使用稳态无自旋进动 (13)C NMR 光谱原位监测电化学反应。
Monitoring electrochemical reactions in situ using steady-state free precession (13)C NMR spectroscopy.
机构信息
Instituto de Química de São Carlos, Universidade de São Paulo, Avenida Trabalhador São-Carlense 400, São Carlos, São Paulo 13560-070, Brazil; Embrapa Instrumentação, Rua XV de Novembro 1452, São Carlos, São Paulo 13560-970, Brazil.
Embrapa Instrumentação, Rua XV de Novembro 1452, São Carlos, São Paulo 13560-970, Brazil; Instituto de Física de São Carlos, Universidade de São Paulo, Avenida Trabalhador São-Carlense 400, São Carlos, São Paulo 13566-590, Brazil.
出版信息
Anal Chim Acta. 2014 Nov 19;850:1-5. doi: 10.1016/j.aca.2014.05.022. Epub 2014 May 20.
All attempts to use in situ(13)C NMR in spectroelectrochemical studies, using static cells and unlabeled substrates, have failed due to the very long average time (several hours). In this paper, we demonstrated that steady-state free precession (SSFP) pulse sequence can enhance signal to noise ratio and reduces the average time of (13)C NMR signals by more than one order of magnitude. The results showed that each (13)C NMR spectrum during the electrochemical reduction of 9-chloroanthracene, in a static cell, can be acquired in eleven minutes. This short averaging time allowed the analysis of the reaction every 30min during 3h. The phase and truncation anomalies present in SSFP spectra were minimized using Traff apodization function and Krylov basis diagonalization method (KBDM).
由于平均时间（数小时）非常长，所有使用静态池和未标记底物进行现场（13）C NMR 光谱电化学研究的尝试都失败了。在本文中，我们证明了稳态自由进动（SSFP）脉冲序列可以增强信噪比，并将（13）C NMR 信号的平均时间降低一个数量级以上。结果表明，在静态池中对 9-氯蒽进行电化学还原期间，每次（13）C NMR 光谱都可以在 11 分钟内采集到。这种短的平均时间允许在 3 小时内每 30 分钟分析一次反应。使用 Traff 削波函数和 Krylov 基对角化方法（KBDM）最小化了 SSFP 光谱中的相位和截断异常。
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