The objective of this work is to compare various extraction and quantitation techniques for the determination of adsorbed polynuclear aromatic hydrocarbons (PAHs) on coal ash. Aliquots of a ＇clean＇ fly ash from coal combustion doped with four PAHs have been extracted, using thr-ee solvents, three methods and three GC/MS programs. Factorial analysis shows solvent to exert the greatest primary effect: CH2Cl2 > toluene much greater than o-xylene. Highest recoveries were obtained using the reflux slurry extraction procedure with CH2Cl2 and a relatively fast (20 degrees/min) temperature ramp to 310 degrees. With both CH2Cl2 and toluene solvents, ultrasonic assisted extraction affords the best repeatability.