Application of Ion Chromatography for the Reliable Quantification of Ammonium in Electrochemical Ammonia Synthesis Experiments: A Practical Guide.

Assessing novel electrocatalysts for the electrochemical ammonia synthesis (EAS) requires reliable quantitative trace analysis of electrochemically produced ammonia to infer activity and selectivity. This study concerns the development of an ion chromatography (IC) method for quantitative trace analysis of ammonium in 0.1 M sulfuric acid electrolyte, which is applied to EAS gas-diffusion electrode (GDE) experiments with commercial chromium nitride as electrocatalyst. The developed IC method is highly sensitive, versatile, and reliable, achieving a limit of quantification (LOQ) of 6 μg l-1 (6 ppbmol ) ammonium. The impacts of the sample matrix, dilution, and neutralization, as well as contamination, on the quantitative analysis by IC are analyzed. Experimental constraints result in an effective LOQ including dilution of 60 μg l-1 for the determination of ammonium in 0.1 M sulfuric acid electrolyte, owing to necessary sample dilution. The practical guide presented herein is intended to be very relevant for the field of EAS as a guideline and applicable to a broad range of catalyst systems and ion chromatography devices. © 2023 The Authors. ChemSusChem published by Wiley-VCH GmbH.

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Sebastian C H Bragulla, Julian Lorenz, Corinna Harms, Michael Wark, K Andreas Friedrich. Application of Ion Chromatography for the Reliable Quantification of Ammonium in Electrochemical Ammonia Synthesis Experiments: A Practical Guide. ChemSusChem. 2023 Jul 07;16(13):e202202211

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PMID: 36929811

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