The comparison of wet digestion and microwave digestion of Cd, Co, Cr,Cu, Mn, Pb, Zn, Fe, and Ni contents of the river bottom and sea floor sedi-ments from the various locations of Turkey was performed in the presentwork. After digestions, the heavy metal concentrations were determinedby flame atomic absorption spectrometry (FAAS). The heating programsfor microwave digestion, different combinations, and volumes of acidmixtures were evaluated for microwave digestion efficiency. Thestudies in the present work show that the microwave-assisted digestions in closed system are easier and faster than the wet digestion. Also theresults found by the microwave and the wet digestions were reliableand accurate. The procedures were also checked with two-stream sedi-ment reference material (GBW 07309 and GBW 07310). Results for stan-dard reference material (SRM) were in good agreement with certifiedvalues.