| Summary: | Research related to measurements of electricity production was combined with parallel wastewater parameter reduction in a membrane-less microbial fuel cell (ML-MFC) fed with industry process wastewater (from a yeast factory). Electrodes with Ni–Co and Cu–B catalysts were used as cathodes. A carbon electrode (carbon cloth) was used as a reference due to its widespread use. It was demonstrated that all analyzed electrodes could be employed as cathodes in ML-MFC fed with process wastewater from yeast production. Electricity measurements during ML-MFC operations indicated that power (6.19 mW) and current density (0.38 mA·cm<sup>−2</sup>) were the highest for Ni–Co electrodes. In addition, during the exploitation of ML-MFC, it was recorded that the chemical oxygen demand (COD) removal per time for all types of electrodes was similar to the duration of COD decrease in the conditions for wastewater aeration. However, the COD reduction curve for aeration took the most favorable course. The concentration of NH<sub>4</sub><sup>+</sup> in ML-MFC remained virtually constant throughout the measurement period, whereas NO<sub>3</sub><sup>−</sup> levels indicated almost complete removal (with a minimum increase in the last days of cell exploitation).
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