The purpose of this paper is to investigate the mineralogical components of palm oil fuel ash (POFA) with or without unburned carbon by using semi-quantitative X-ray diffraction (XRD). Original POFA taken from palm oil mill was ground in ball mill, producing ground POFA (GPOFA). Unburned carbon was removed by heating the GPOFA at 500 °C for 1 h, producing treated POFA (TPOFA). Neither glassy phase crystallization nor agglomeration of GPOFA particles occurred during the heat treatment. The content of crystalline phase and glassy phase in GPOFA or TPOFA was determined using semi-quantitative XRD analysis internal standard method. The results showed that GPOFA and TPOFA contained 67.22% and 73.89% of glassy phase, respectively, which could be used as pozzolanic materials. The presence of P2O5, K2O and Na2O in POFA was the reason of reducing the melting point of POFA in boiler.