Studies on leaching behavior of metals associated with coal fly ash (FA) are of great concern because of possible contamination of the aquatic environment. In the present study, leaching behavior of metals (As, Se, Cr, Pb, V, Zn, etc.) in two different FA samples (FA1 and FA2) was investigated at various pH (2–12), temperatures of leachate solution and using TCLP. At pH 2, the highest leaching was observed for Fe (21.6 and 32.8 µg/g), whereas at pH 12, Arsenic was found to have the highest leaching (1.5 and 2.4 µg/g) in FA1 and FA2. Leachate solution temperature showed a positive effect on the metal’s leachability. In TCLP, most of the metal’s leachability was observed to be higher than that of batch leaching tests. The present study suggests that, leaching of As and Se from FA samples can moderately affect ground/surface water quality at the study locations.