Legion: An Instrument for High-Throughput Electrochemistry

Abstract

Electrochemical arrays promise utility for accelerated hypothesis testing and breakthrough discoveries. Herein, we report a new high-throughput electrochemistry platform, colloquially called "Legion," for applications in electroanalysis and electrosynthesis. Legion consists of 96 electrochemical cells dimensioned to match common 96-well plates that are independently controlled with a fieldprogrammable gate array. We demonstrate the utility of Legion by measuring model electrochemical probes, pH-dependent electron transfers, and electrocatalytic dehalogenation reactions. We consider advantages and disadvantages of this new instrumentation, with the hope of expanding the electrochemical toolbox.

Nanomaterials Synthesis Discovery via Parallel Electrochemical Deposition

“…The 12 eight-channel potentiostat boards interface with a field programmable gate array (FPGA) and custom software, enabling independent control of the QRCE in each well. Additional details about the Legion instrument design can be found in ref ( 17 ).…”

“…This enables development of electrochemical synthesis and discovery with an experimental bandwidth equivalent to colloidal synthesis. We enable discovery with a multichannel potentiostat recently described by Gerroll et al, 17 colloquially referred to as “Legion.” Designed around the footprint of a 96-well plate, Legion uses a single, large working electrode (WE) and 96 quasi-reference counter electrodes (QRCEs) to conduct 96 parallel electrochemical experiments, each in one of the 96 separate wells. Instrument control by a field programmable gate array (FPGA) enables independent variation of both the chemical and electrochemical parameters in each well.…”

Autonomous closed-loop mechanistic investigation of molecular electrochemistry via automation

“…There have been key developments in high-throughput experimentation hardware for synthetic purposes 12 – 17 that can be translated to electrochemical research 18 – 24 , yet additional automated electroanalytical platforms with minimized adoption barriers are needed for fundamental mechanistic investigations. Customized multi-well parallel-plate reactors 18 – 22 have been reported for evaluating organic electrosynthesis, and microfabricated microfluidic devices 23 , 24 have been reported for automated electrokinetic measurements. Nevertheless, there remains a need for automated experimentation platforms with minimized barriers to entry that resemble standard electroanalytical setups in a typical laboratory, in order to directly utilize the vast tools available to electrochemists to obtain mechanistic information 8 – 11 .…”

Interfacing High-Throughput Electrosynthesis and Mass Spectrometric Analysis of Azines

“…■ EXPERIMENTAL SECTION Legion HTE. Instrument design of Legion is previously reported by Gerroll et al 24 Each well is an individual electrochemical cell with a two-electrode configuration. The working electrode is a glassy carbon plate or graphite plate (redox.me) with an exposed electroactive surface area of 38.5 mm 2 per well.…”

“…We have recently described a platform for high-throughput electrochemistry, called "Legion," which is capable of simultaneous, individual, arrayed electrochemical measurements across all electrochemical cells. 24 Moreover, to facilitate complementary analysis tools such as MS, the footprint of Legion is modeled after a commercial 96-well microtiter plate.…”