Discovery of electrocatalytic materials for high-performance energy conversion and storage applications relies on the adequate characterization of their intrinsic activity, which is currently hindered by the dearth of a protocol for consistent and precise determination of double layer capacitance (C _DL). Herein, we propose a seven-step method that aims to determine C _DL reliably by scan rate-dependent cyclic voltammetry considering aspects that strongly influence the outcome of the analysis, including (a) selection of a suitable measuring window, (b) the uncompensated resistance, (c) optimization of measuring settings, (d) data acquisition, (e) selection of data suitable for analysis, (f) extraction of the desired information, and (g) validation of the results. To illustrate the proposed method, two systems were studied: a resistor–capacitor electric circuit, and a glassy carbon disk in an electrochemical cell. With these studies, it is demonstrated that when any of the mentioned steps of the procedure are neglected, substantial deviations of the results are observed with misestimations as large as 61% in the case of the investigated electrochemical system. Moreover, we propose allometric regression as a more suitable model than linear regression for the determination of C _DL for both the ideal and the non-ideal systems investigated. We stress the importance of assessing the accuracy of not only highly specialized electrochemical methods, but also of those that are well-known and commonly used as it is the case of the voltammetric methods. The procedure proposed herein is not limited to the determination of C _DL, but can be effectively applied to any other analysis that aims to deliver quantitative results via voltammetric methods, which is crucial for the study of kinetic and diffusion phenomena in electrochemical systems.

用于高性能能量转换和存储应用电催化材料的发现依赖于它们的固有活性，目前由用于双层电容（一致和精确地确定一个协议的缺乏阻碍了充分的表征Ç _DL）。在此，我们提出了一种旨在确定C _{DL 的}七步方法考虑到强烈影响分析结果的方面，包括 (a) 选择合适的测量窗口，(b) 未补偿的电阻，(c) 优化测量设置，(d) 数据采集, (e) 选择适合分析的数据，(f) 提取所需信息，以及 (g) 结果验证。为了说明所提出的方法，研究了两个系统：电阻-电容器电路和电化学电池中的玻璃碳盘。通过这些研究，证明当忽略该过程中提到的任何步骤时，观察到结果的显着偏差，在所研究的电化学系统的情况下，错误估计高达 61%。而且，研究 了理想和非理想系统的C _DL。我们强调不仅要评估高度专业化的电化学方法的准确性，还要评估那些众所周知和常用的方法的准确性，就像伏安法一样。本文提出的程序不仅限于C _DL的测定，而且可以有效地应用于旨在通过伏安法提供定量结果的任何其他分析，这对于研究电化学系统中的动力学和扩散现象至关重要。