Accurate analysis of fly ash particles is not trivial because of complex nature in physical and chemical properties. SPLITT fractionation (SF) was employed to fractionate the fly ash particles into subpopulations in large quantities. Then the SF-fractions were analyzed by the steric mode of sedimentation field-flow fractionation (Sd/StFFF) for size analysis. The SF-fractions were also analyzed by ICP-OES. The results showed that the fly ash is mainly composed of Fe, Ca, Mg and Mn. No particular trends were observed between the particle size and the concentrations of Fe, Ca, Mg, while Mn, Cu and Zn were in higher concentrations in smaller particles. Sample preparation procedures were established, where the fly ash particles were sieved to remove large contaminants, and then washed with acetone to remove organics on the surface of particles. The sample preparation and analysis methods developed in this study could be applied to other environmental particles.