Unveiling the quantification minefield in electrocatalytic urea synthesis

Huang, Yanmei; Wang, Yuting; Liu, Yang; Ma, Aiyuan; Gui, Jianzhou; Zhang, Chaoxin; Yu, Yifu; Zhang, Bin

doi:10.1016/j.cej.2022.139836

Cited by 38 publications

(36 citation statements)

References 37 publications

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“…The diacetyl monoxime method is a method for measuring urea concentration by analyzing the colorimetric product formed by the reaction between urea and diacetyl monoxime in the presence of ferric chloride and thiosemicarbazide under acidic electrolyte conditions. 36 The concentration of this chromogenic product is proportional to the UV−vis absorbance at wavelengths of 520−530 nm, and the urea content can be determined using UV−vis absorption spectroscopy. 21 Zhang and colleagues found that the limit of detection for this method was 0.26 ppm in pure H 2 O and 0.14 ppm in 0.2 M KHCO 3 electrolyte.…”

Section: Discussionmentioning

confidence: 99%

“…21 Zhang and colleagues found that the limit of detection for this method was 0.26 ppm in pure H 2 O and 0.14 ppm in 0.2 M KHCO 3 electrolyte. 36 Moreover, the accuracy of this method can be affected by certain interference factors, such as the presence of high concentrations of NO 2 − . Specifically, when the concentration of NO 2 − is below 20 ppm, the relative error for urea determination is within ±7.5%.…”

Section: Discussionmentioning

confidence: 99%

“…Zhang's group demonstrated that the detection limit of the urease decomposition method for measuring urea concentration is 0.52 ppm in 0.2 M KHCO 3 electrolyte. 36 They also studied the potential interference factors on the accuracy of this method, including the effects of NO 2 − and NH 4 + . Specifically, NO 2 − can suppress the formation of the indophenol derivative, leading to an underestimation of generated NH 4 + and a lower calculated urea concentration.…”

Section: Discussionmentioning

confidence: 99%

“…The detection limit of this method is 0.54 ppm in 0.2 M KHCO 3 electrolyte. 36 Moreover, the presence of metal ions or by-products has no obvious effect on the quantification of urea by the 1 H NMR spectroscopy method, owing to the difference in the chemical environment of hydrogen atoms. 43 The detection limit of the HPLC method is 0.42 ppm in a 0.2 M KHCO 3 electrolyte to measuring urea concentration.…”

mentioning

confidence: 99%

“…Furthermore, the presence of the C-containing (HCOO − , CH 3 OH, and CH 3 CH 2 OH), Ncontaining (NH 4 + , NO 2 − , and NO 3 − ), and other C−N coupling by-products (such as formamide and acetamide) has no obvious interference to the quantification of urea by the HPLC method. 36 At present, 1 H NMR spectroscopy and HPLC could be relatively reliable methods for measuring the amount of urea. Additionally, due to the low concentrations of urea in electrochemical studies, it is necessary to conduct isotope-labeled control experiments to confirm that the urea is derived from the electrochemical reduction of CO 2 and nitrogenous compounds, rather than being contaminated by impurities.…”

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confidence: 99%

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Review on Electrocatalytic Coreduction of Carbon Dioxide and Nitrogenous Species for Urea Synthesis

et al. 2023

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The electrochemical coreduction of carbon dioxide (CO 2 ) and nitrogenous species (such as NO 3 − , NO 2 − , N 2 , and NO) for urea synthesis under ambient conditions provides a promising solution to realize carbon/nitrogen neutrality and mitigate environmental pollution. Although an increasing number of studies have made some breakthroughs in electrochemical urea synthesis, the unsatisfactory Faradaic efficiency, low urea yield rate, and ambiguous C−N coupling reaction mechanisms remain the major obstacles to its large-scale applications. In this review, we present the recent progress on electrochemical urea synthesis based on CO 2 and nitrogenous species in aqueous solutions under ambient conditions, providing useful guidance and discussion on the rational design of metal nanocatalyst, the understanding of the C−N coupling reaction mechanism, and existing challenges and prospects for electrochemical urea synthesis. We hope that this review can stimulate more insights and inspiration toward the development of electrocatalytic urea synthesis technology.

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Section: Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

Section: Discussionmentioning

confidence: 99%

mentioning

confidence: 99%

mentioning

confidence: 99%

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Review on Electrocatalytic Coreduction of Carbon Dioxide and Nitrogenous Species for Urea Synthesis

et al. 2023

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Urea Electrosynthesis Accelerated by Theoretical Simulations

Liu,

Guo,

Frauenheim

et al. 2023

Adv Funct Materials

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Urea is not only a primary fertilizer in modern agriculture but also a crucial raw material for the chemical industry. In the past hundred years, the prevailing industrial synthesis of urea heavily relies on the Bosch–Meiser process to couple NH3 and CO2 under harsh conditions, resulting in high carbon emissions and energy consumption. The conversion of carbon‐ and nitrogen‐containing species into urea through electrochemical reactions under ambient conditions represents a sustainable strategy. Despite the increasing reports on urea electrosynthesis, a comprehensive review that delves into a profound, atomic‐level comprehension of the fundamental reaction mechanisms is currently absent. In this Perspective, recent advancements in electrochemical urea synthesis from CO2/CO and various nitrogenous species (i.e., N2, NOx−, and NO) under ambient conditions are presented, with special emphasis on theoretical understanding of the C─N coupling reaction mechanisms. Several key strategies to facilitate the C─N coupling are then pinpointed, which not only enhance their applicability in practical experiments but also highlight the significant progress achieved in this field. At the end, the major obstacles and potential opportunities in advancing urea electrosynthesis accelerated by theoretical simulations and in situ techniques are discussed. This review is hoped to act as a roadmap to ignite fresh insights and inspiration for the development of electrocatalytic urea synthesis.

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Fundamentals and Rational Design of Heterogeneous C‐N Coupling Electrocatalysts for Urea Synthesis at Ambient Conditions

Wan,

Zheng,

Yan

et al. 2024

Advanced Energy Materials

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Electrocatalytic C‐N coupling reaction is regarded as a promising strategy for achieving clean and sustainable urea production by coreducing CO2 and nitrogen species, thus contributing to carbon neutrality and the artificial nitrogen cycle. However, restricted by the sluggish adsorption of reactants, competitive side reactions, and multistep reaction pathways, the electrochemical urea production suffers from a low urea yield rate and low selectivity so far. In order to comprehensively improve urea synthesis performance, it is crucial to develop highly efficient catalysts for electrochemical C‐N coupling. In this article, the catalyst‐designing strategies, C‐N coupling mechanisms, and fundamental research methods are reviewed. For the coreduction of CO2 and different nitrogen species, several prevailing reaction mechanisms are discussed. With the aim of establishing the standard research system, the fundamentals of electrocatalytic urea synthesis research are introduced. The most important catalyst‐designing strategies for boosting the electrocatalytic urea production are discussed, including heteroatom doping, vacancy engineering, crystal facet regulation, atom‐scale modulation, alloying and heterostructure construction. Finally, the challenges and perspectives are proposed for future industrial applications of electrochemical urea production by C‐N coupling.

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Unveiling the quantification minefield in electrocatalytic urea synthesis

Cited by 38 publications

References 37 publications

Review on Electrocatalytic Coreduction of Carbon Dioxide and Nitrogenous Species for Urea Synthesis

Review on Electrocatalytic Coreduction of Carbon Dioxide and Nitrogenous Species for Urea Synthesis

Urea Electrosynthesis Accelerated by Theoretical Simulations

Fundamentals and Rational Design of Heterogeneous C‐N Coupling Electrocatalysts for Urea Synthesis at Ambient Conditions

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