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加速核磁共振氢谱对氨水的检测

Accelerating H NMR Detection of Aqueous Ammonia.

作者信息

Kolen Martin, Smith Wilson A, Mulder Fokko M

机构信息

Materials for Energy Conversion and Storage (MECS), Department of Chemical Engineering, Delft University of Technology, Van der Maasweg 9, 2629 HZ Delft, The Netherlands.

出版信息

ACS Omega. 2021 Feb 19;6(8):5698-5704. doi: 10.1021/acsomega.0c06130. eCollection 2021 Mar 2.

Abstract

Direct electrolytic N reduction to ammonia (NH) is a renewable alternative to the Haber-Bosch process. The activity and selectivity of electrocatalysts are evaluated by measuring the amount of NH in the electrolyte. Quantitative H nuclear magnetic resonance (qNMR) detection reduces the bench time to analyze samples of NH (present in the assay as NH ) compared to conventional spectrophotometric methods. However, many groups do not have access to an NMR spectrometer with sufficiently high sensitivity. We report that by adding 1 mM paramagnetic Gd ions to the NMR sample, the required analysis time can be reduced by an order of magnitude such that fast NH detection becomes accessible with a standard NMR spectrometer. Accurate, internally calibrated quantification is possible over a wide pH range.

摘要

直接电解将氮气还原为氨是哈伯-博施法的一种可再生替代方法。通过测量电解液中氨的含量来评估电催化剂的活性和选择性。与传统分光光度法相比,定量氢核磁共振(qNMR)检测减少了分析氨样品(在分析中以铵离子形式存在)的实验时间。然而,许多研究团队无法使用灵敏度足够高的核磁共振光谱仪。我们报告称,通过向核磁共振样品中添加1 mM顺磁性钆离子,所需的分析时间可减少一个数量级,从而使用标准核磁共振光谱仪就能实现快速氨检测。在很宽的pH范围内都可以进行准确的、内部校准的定量分析。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/ff78/7931439/bd38ecb70453/ao0c06130_0002.jpg

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