Thirty elements are determined in coal and fly ash by instrumental neutron-activation analysis using both thermal and epithermal irradiation. Gamma-ray spectra were recorded 7 and 20 days after the irradiations. The procedure is applicable to the routine analysis of coals and fly ash. Epithermal irradiation was found preferable for the determination of Ni, Zn, As, Se, Br, Rb, Sr, Mo, Sb, Cs, Ba, Sm, Tb, Hf, Ta, W, Th and U, whereas thermal irradiation was best for Sc, Cr, Fe, Co, La, Ce, Nd, Eu, Yb and Lu. Results for SRM 1632 (coal) and SRM 1633 (fly ash) agree with those of other investigators. ?? 1977.