A method for the determination of sulphur in fly ash by instrumental proton activation analysis using the34S/p,n/34mCl reaction was developed. The 2128.5 keV and 3305.0 keV -rays of34mCl /t=32.0 min/ were measured on a Ge/Li/ -spectrometer, shielded with a lead absorber to attenuate low energy -rays. Irradiation and measuring conditions were optimized. The detection limit for instrumental analysis is 0.3 to 1 mg g–1 and the standard deviation is cca. 4% for a typical sample.