Biocharcoal (BioC), a cost-effective, eco-friendly, and sustainable material can be derived from various organic sources including agricultural waste. However, to date, complex chemical treatments using harsh solvents or physical processes at elevated temperatures have been used to activate and enhance the functional groups of biochar. In this paper, we propose a novel easy and cost-effective activation method based on electrochemical cycling in buffer solutions to enhance the electrochemical performance of biocharcoal derived from almond shells (AS-BioC). The novel electrochemical activation method enhanced the functional groups and porosity on the surface of AS-BioC, as confirmed by microscopic, spectroscopic characterizations. Electrochemical characterization indicated an increase in the conductivity and surface area. A modified SPCE with activated AS-BioC (A.AS-BioC/SPCE), shows enhanced electrochemical performance towards oxidation and reduction of nitrite and paraxon ethyl pesticide, respectively. For both target analytes, the activated electrode demonstrates high electrocatalytic activity and achieves a very LOD of 0.38 µM for nitrite and 1.35 nM for ethyl paraxon with a broad linear range. The sensor was validated in real samples for both contaminants. Overall, the research demonstrates an innovative technique to improve the performance of AS-BioC to use as a modifier material for electrochemical sensors.