We report a method for rapid screening of arrays of electrocatalyst candidates. The approach is based on simultaneous activation of the oxygen reduction reaction (ORR) and Ag electrodissolution at the cathodic and anodic poles, respectively, of bipolar electrodes (BPEs). Because the electrochemical activity of the two poles is directly coupled via the BPE, the extent of Ag electrodissolution is directly related to the ORR activity. The screening process lasts ∼12 min. Because Ag dissolution provides a permanent record of catalyst activity, the screening results can be determined by simple optical microscopy after the electrochemical experiment. The method has the potential to provide quantitative information about electrocatalyst activity.H ere we report a new and potentially powerful method for rapid screening of electrocatalysts. The principle is illustrated in Scheme 1, with specific reference to evaluation of the activity of electrocatalysts for the oxygen reduction reaction (ORR). The top frame of Scheme 1a shows an array of three bipolar electrodes (BPEs). 1 The ORR electrocatalyst candidates are deposited onto the cathodic poles of the BPEs, while the anodic poles are composed of parallel Ag microband electrodes. The Ag microbands of each electrode are in electrical contact with one another and with the ORR catalyst via an underlying indium-doped tin oxide (ITO) contact. When a sufficiently high potential (E tot , Scheme 1b) is applied to the solution in the fluidic channel via a pair of driving electrodes, the ORR proceeds at the cathodic poles and the Ag microbands undergo electrodissolution. 2 The efficiency of the ORR catalyst is then determined by counting the number of dissolved Ag microband electrodes: the more bands that dissolve, the better the catalyst. In fact, as we will show, there is a direct thermodynamic link between the overpotential required for the ORR (Scheme 1c) and the number of Ag microbands remaining after the experiment (Scheme 1a). Although we demonstrate this screening method using just three BPEs, arrays of arbitrary size can be monitored in this way with very little additional technological overhead. This is because it is not necessary to make a direct electrical connection to each electrode, which is an intrinsic property of BPEs and the principal reason for using them in an array format. 3 The basic operating principles of BPEs, along with many interesting applications, have been previously described in the scientific literature. 1−14 A driving voltage E tot applied across a microchannel containing a conductive electrolyte solution (Scheme 1b) is dropped nearly linearly over the length of the microchannel. 6 If a conductive wire of sufficient length is present in the microchannel, it will function as a BPE. 1 Specifically, when the interfacial potential differences between the poles of the BPE and the electrolyte solution (ΔE elec , Scheme 1a) are sufficiently high, faradaic processes occur simultaneously: a reduction at the cathodic pole and an oxidation at the a...