Kolen Martin, Smith Wilson A, Mulder Fokko M
Materials for Energy Conversion and Storage (MECS), Department of Chemical Engineering, Delft University of Technology, Van der Maasweg 9, 2629 HZ Delft, The Netherlands.
ACS Omega. 2021 Feb 19;6(8):5698-5704. doi: 10.1021/acsomega.0c06130. eCollection 2021 Mar 2.
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.
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。