The article introduced a analytical method of heavy metal fractions in soil and sediment. Heavy metals in soil and sediment were divided into five fractions: water soluble, acid extractable, reducible, oxidizable and residual. They were extracted respectively by water, 0.11mol/L acetic acid, 0.5mol/L hydroxyamine hydrochloride, hydrogen peroxide and 1.0 mol/L ammonium acetate, and hydrochloric acid-nitric acid- hydrofluoric-perchloric acid. It was adapted to special analyses of heavy metals including Cu, Pb, Zn, Cd, Cr, Co, Mn, Mo, As, Sb and Ni. The detection limit were 0.001 ~ 1 μg/g. The precision test were less than 11% RSD (n = 4).