Easily Constructed Microscale Spectroelectrochemical Cell.

The design and performance of an easily constructed cell for microscale spectroelectrochemical analysis is described. A cation exchange polymer film, Nafion, was used as a salt bridge to provide ionic contact between a small sample well containing a coiled wire working electrode and separate, larger wells housing reference and auxiliary electrodes. The cell was evaluated using aqueous ferri/ferrocyanide as a test system and shown to be capable of relatively sensitive visible absorption measurements (path lengths on the order of millimeters) and reasonably rapid bulk electrolysis (~ 5 min) of samples in the 1 to 5 μL volume range. Minor alterations to the cell design are cited that could allow for analysis of sub-microliter volumes, rapid multi-sample analysis, and measurements in the ultraviolet spectral region.