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<sub>DL</sub>).
Herein, we propose a seven-step method that aims to determine C<sub>DL</sub>
reliably by scan rate-dependent cyclic voltammetry. The method considers three
aspects that strongly influence the outcome of the analysis: measurement
settings, data collection, and data processing. 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 aspects 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<sub>DL</sub> 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
methodology proposed herein is not limited to the determination of C<sub>DL</sub>,
but can be effectively applied to any other voltammetry-based analysis that
aims to deliver quantitative results.