<p>The levels of natural radioactivity in coal and coal combustion residues from three coal-fired power plants in Pakistan were determined. This pioneering study will serve as a basis to develop national regulations for activities involving Naturally Occurring Radioactive Material (NORM). Gamma Spectrometry was used to measure activity levels of ²³⁸U, ²²⁶Ra, ²³²Th, and ⁴⁰K in raw coal, fly ash, and bottom ash, followed by estimation of radiological risk parameters. The results were below the standard limits. Routine monitoring of ash samples was recommended, particularly before their sale, reuse, transport, handling, and disposal, as risk parameter levels approached the limits.</p>