Analytical chemists frequently receive samples that cannot be analyzed in the natural state, due to the presence of interferences and/or inadequate sensibility of the available analytical methodology. Previous steps for separation and enrichment are almost always necessary, and many procedures have been proposed. The process, involving extraction in solid phase, has received more acceptance due to a number of possible advantages, including the availability and easy recovery of the solid phase, attainability of large preconcentration factors and the facility for separation and enrichment using systems with continuous flow. Besides, they usually do not need organic solvents, which may be toxic. For cobalt adsorption determination, several procedures have been proposed involving polyurethane foam 1 , activated carbon 2,3 , Amberlite XAD-4 resin 4,5 , naphthalene 6 and C 18 -bonded silica gel column; 7,8 other techniques as coprecipitation using indium hydroxide as colector 9 , liquid-liquid extraction 10 and cobalt separation as complex and filtration with a menbrane filter.