Leakless, Bipolar Reference Electrodes: Fabrication, Performance, and Miniaturization.
Leakless, Bipolar Reference Electrodes: Fabrication, Performance, and Miniaturization.
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DOI：
10.1021/acs.analchem.1c00675
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发表时间：
2021-07-27
影响因子：
7.4
通讯作者：
Dick, Jeffrey E.
中科院分区：
文献类型：
--
作者：
Walker, Nicole L.;Dick, Jeffrey E.
参比电极必须长时间保持明确的电位才能使用。银/氯化银（Ag/AgCl）参比电极可以说是最广泛使用的参比电极，但随着时间的推移，银和氯离子会通过多孔玻璃料泄漏到样品溶液中。此外，多孔玻璃料使得微型化到微米和纳米级具有挑战性。在这里，我们提出了一种替代方案，其中传统的Ag/AgCl参比电极多孔玻璃料被导电线取代，防止离子泄漏，并允许微型化到微米级。电荷平衡通过封闭的双极电化学机制来维持，其中法拉第过程发生在密封导线的每一端。使用上述设计，我们证明了无泄漏双极参比电极（BPRE）的有效性，并将其扩展到微尺度（μ-无泄漏BPRE）。重要的是，我们证明了无泄漏和μ-无泄漏的BPRE在电位测量期间与商业参比电极的行为相同，并且无泄漏的BPRE在超微电极上的伏安测量期间表现相似。我们证明，在伏安法使用无泄漏的BPRE在宏电极的漂移是稍微更明显的漂移相比，看到一个商业参考电极。我们详细介绍了在非水溶剂中使用无泄漏BPRE和密封其他导电材料（例如，金和碳）。使用质谱，我们表明，亚甲蓝的最大泄漏为0.36 fmol/s，至少2个数量级小于商业参比电极。最后，我们证明了在电位葡萄糖传感中使用无泄漏BPRE的功效。
Reference electrodes must maintain a well-defined potential for long periods of time to be useful. The silver/silver chloride (Ag/AgCl) reference electrode is arguably the most widely used reference electrode, but it leaks silver and chloride ions into the sample solution through the porous frit over time. Further, the porous frit makes miniaturization to the micro- and nanoscale challenging. Here, we present an alternative, where the traditional Ag/AgCl reference electrode porous frit is replaced by a conductive wire, preventing ion leakage and allowing miniaturization to the microscale. Charge balance is maintained through a closed bipolar electrochemical mechanism, where faradaic processes occur on each end of the sealed wire. Using the above design, we demonstrate the efficacy of the leakless, bipolar reference electrode (BPRE) and miniaturize it to the microscale (μ-leakless BPRE). Importantly, we demonstrate that leakless and μ-leakless BPREs behave the same as commercial reference electrodes during potentiometric measurements and leakless BPREs perform similarly during voltammetric measurements on ultramicroelectrodes. We demonstrate that the drift during voltammetry using a leakless BPRE on a macroelectrode is slightly more appreciable compared to the drift seen with a commercial reference electrode. We detail design principles for the use of leakless BPREs in nonaqueous solvents and in sealing other conductive materials (e.g., gold and carbon). Using mass spectrometry, we show that the maximum leakage of methylene blue is 0.36 fmol/s, at least 2 orders of magnitude smaller than that of commercial reference electrodes. Finally, we demonstrate the efficacy of using leakless BPREs in potentiometric glucose sensing.
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