The current research was investigated the mechanism of coal demineralization and the effect of leaching parameters on high ash coal and study the characterization of pre and post-treated coal. The two high ash Indian coal selected from Mahanadi Coalfield Limited, Odisha, pulverized to 375, 230 and 180 lm particle size were undergone simultaneous acid and alkali treatment at a different concentration, temperature and time. The percent demineralization was increased with decrease the size of the particle and rises with leaching parameters. The investigation suggested 180 lm particle size offers efficient demineralization for both coals at 30% NaOH and 30% H 2 SO 4 concentration. The alkali leaching leads to obtaining the demineralization 46% and 42% whereas acid treatment resulted in 34% and 32% of the original coal samples. The extent of demineralization was improved the calorific value of coal. Besides, the degree of demineralization was proved from the FTIR, XRF and FESEM-EDX analysis results. FTIR analysis result showed that the peak intensity of mineral band decreased by the leaching effect and the degree of demineralization was significantly obtained to large extent by the X-ray Fluorescence spectrometer; which elucidates major minerals removed from coal by the leaching effect of acid and alkali solution.