This review presents the most recent applications of solid phase extraction for the separation, preconcentration and speciation of metals, metalloids, and organometals. The review focuses on solid phase, column treatments and on the applications of this technique to various samples. This review also intends to discuss some applications and limitations associated to solid phase extraction techniques due to the necessity on limited selectivity. Nevertheless, the solid phase extraction is still an efficient, sensitive and inexpensive technique to perform removal of metal ions from environmental samples, preconcentration of metal ions for analytical purposes and speciation of the metal and metalloids as shown by the variety of applications presented and discussed in this review. A literature survey of the last three years (2008-2010) offering a critical review of solid phase extraction for separation, preconcentration and speciation of metal ions from various sample matrices is provided.