Versatile 3D‐Printed Micro‐Reference Electrodes for Aqueous and Non‐Aqueous Solutions

Schuett, Fabian M.; Zeller, Sven; Eckl, Maximilian J.; Matzik, Felix M.; Heubach, Maren-Kathrin; Geng, Tanja; Hermann, Johannes M.; Uhl, Matthias; Kibler, Ludwig A.; Engstfeld, Albert K.; Jacob, Timo

doi:10.1002/anie.202105871

Cited by 7 publications

(8 citation statements)

References 55 publications

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“…The reference electrode, which is a self‐made 1 m Cu/CuCl 2 micro‐reference electrode, is placed from the side and the Au(111) single crystal can be dipped from atop, forming a hanging meniscus. The whole setup is installed in a glass tube with screwable caps for the top and bottom to reduce contaminations during the measurement [42] . The aqueous measurement was carried out using an SP‐300 Potentiostat from BioLogic and the same cell outside of the glovebox.…”

Section: Methodsmentioning

confidence: 99%

“…The whole setup is installed in a glass tube with screwable caps for the top and bottom to reduce contaminations during the measurement. [42] The aqueous measurement was carried out using an SP-300 Potentiostat from BioLogic and the same cell outside of the glovebox. The electrolyte and the glass tube containing the cell were purged with N 2 for 1 h before the measurement to get rid of O 2 in the system.…”

Section: Electrochemical Cellsmentioning

confidence: 99%

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An Interfacial Study of Au(111) Electrodes in Deep Eutectic Solvents

et al. 2022

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The electrochemical behavior of Au(111) in contact with deep eutectic solvents (DESs) was studied by cyclic voltammetry, electrochemical impedance spectroscopy (EIS), and immersion experiments to determine the potential of zero total charge (pztc). In particular, DESs type III consisting of a choline salt and a hydrogen bond donor (HBD) were investigated. The HBDs urea and ethylene glycol (EG) were chosen since they belong, in combination with choline chloride (ChCl), to the most widely studied systems. A third HBD used in this study was trifluoroacetamide (TFAcA) because of its remarkable freezing point depression. The adsorption of chloride, nitrate, and sulfate anions on Au(111) was investigated using DESs, as the electrochemical behavior of Au(111) in aqueous electrolytes containing these anions were already well studied. For a better understanding of the interactions of ions in DESs with noble metal electrode surfaces, Au(111) in aqueous ChCl was investigated as well. It was shown that anion adsorption on Au(111) in the DESs under consideration was similar to adsorption in the respective dilute aqueous systems.

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Section: Methodsmentioning

confidence: 99%

Section: Electrochemical Cellsmentioning

confidence: 99%

An Interfacial Study of Au(111) Electrodes in Deep Eutectic Solvents

et al. 2022

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“…99 Schuett et al offered a straightforward approach for fabricating 3D-printed micro-reference electrodes (Figure 4b). 100 The chemically…”

Section: Miniaturization Of Screening Devicesmentioning

confidence: 99%

“…99 Schuett et al offered a straightforward approach for fabricating 3D-printed micro-reference electrodes (Figure 4b). 100 The chemically resistant polyvinylidene fluoride was used to 3D print the micro-reference electrodes (REs), which have an outer diameter of 4 mm and a length of 40 mm. The electrodes are sealed with a magnesia stick to ensure sealing.…”

Section: Short Review Synthesismentioning

confidence: 99%

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Accelerated Electrosynthesis Development Enabled by High-Throughput Experimentation

Chen

2023

Synthesis

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Electrochemical synthesis has recently emerged as an environmentally benign method for synthesizing value-added fine chemicals. Its unique reactivity has attracted significant interests of synthetic chemists to develop new redox chemistries. However, compared to conventional chemistry, the increased complexity caused by electrode materials, supporting electrolytes, and setup configurations create obstacles for efficient reaction discovery and optimization. The recent increasing adoption of high-throughput experimentation (HTE) in synthetic chemistry significantly expedites the synthesis development. Considering the potential of implementing HTE in electrosynthesis to tackle the challenges of increased parameter space, this short review aims at providing recent advances in the HTE technology for electrosynthesis, including electrocatalysts screening, device miniaturization, electroanalytical methods, artificial intelligence, and system integration. The discussed contents also cover some topics in HTE electrochemistry for areas other than synthetic chemistry, hoping to spark some inspirations for readers to use interdisciplinary techniques to solve challenges in synthetic electrochemistry.

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Construction and Evaluation of Cheap and Robust Miniature Ag/AgCl Reference Electrodes for Aqueous and Organic Electrolytes

Lyu,

Mollik,

Oláh

et al. 2024

ChemElectroChem

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Stable reference electrodes (REs) are crucial for reliable voltammetry, controlled potential electrosynthesis, or spectro‐electrochemistry. Yet, inferior pseudo‐REs, such as plain Ag wire are often used, because commercial REs are expensive, may degrade or contaminate under required conditions, or don't fit geometric restrictions of custom setups. Addressing such cases, we report construction, benchmarking and utilization of easy to make, cheap (<1 €), and robust miniature REs from pasteur pipettes, molecular sieve beads and Ag wire. Excellent potential precision and accuracy with at least 1 week device stability was obtained for aqueous Ag/AgCl REs with 3 M NaCl in H2O and anhydrous 0.1 M TBACl in MeCN inner‐electrolytes. Even in alkaline 1 M NaOH electrolyte, where initial Ag/AgCl REs quickly convert to Ag/Ag2O (1 M NaOH) REs, perfect potential precision, accuracy, and at least 1 week stability are demonstrated. According to experimental needs, miniature REs can be built with many organic and aqueous electrolytes. For these custom use‐cases, we report guidelines to calibrate absolute RE potential, and to assess device precision, accuracy and stability. Finally, electro‐hydrogenation of styrene on nickel electrodes exemplifies superiority of Ag/AgCl REs over Ag wire pseudo‐REs, affording more reliable electrolysis current, cell potential and potential dependent Faraday efficiency.

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Versatile 3D‐Printed Micro‐Reference Electrodes for Aqueous and Non‐Aqueous Solutions

Cited by 7 publications

References 55 publications

An Interfacial Study of Au(111) Electrodes in Deep Eutectic Solvents

An Interfacial Study of Au(111) Electrodes in Deep Eutectic Solvents

Accelerated Electrosynthesis Development Enabled by High-Throughput Experimentation

Construction and Evaluation of Cheap and Robust Miniature Ag/AgCl Reference Electrodes for Aqueous and Organic Electrolytes

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