Oil palm kernel shell ash (POFA), a byproduct of the highly cultivated agro-industrial sector in Colombia, has been widely used for its pozzolanic properties, which enhance the mechanical and durability characteristics of concrete. Six POFA samples were analyzed after undergoing drying, cutting, grinding, crushing, and calcination at temperatures ranging from 500 °C to 1000 °C. SEM-EDS/EDX analysis, X-ray fluorescence (XRF), and loss on ignition (LOI) tests were conducted to characterize its pozzolanic potential. The results revealed that the SiO2 content increased with the calcination temperature, reaching a peak of 76.8% at 1000 °C. However, calcination at 600 °C was identified as the optimal temperature, as it balances impurity removal without inducing the formation of crystalline silica, which would negatively affect the material’s reactivity. Considering the optimal calcination temperature and the high initial LOI values, which exceeded 70% in the first calcination stage, a second calcination was performed on the 500 °C sample by increasing the temperature to 600 °C. This resulted in an LOI of 3.33%, according to ASTM C311 standards for natural pozzolans used in Portland cement concretes.