At this thesis, two novel, simple, sensitive and effective methods for preconcentration and separation of copper ion is presented. The methods has been developed for selective extraction and pre-concentration of copper with N,N-(4-methyl-1,2-phenylene)diquinoline-2carboxamide (Mebqb) as a ligand that immobilized on the naphthalene and graphite. Under the optimum conditions, the copper ions in aqueous samples were separated and preconcentrated by the column. After preconcentration, copper was eluted from sorbent by suitable elution. Flame atomic absorption spectrometry (FAAS) was used for determination of copper ions in eluted solutions. The effect of pH, sample flow rate and the volume, concentration and flow rate of eluent on the recovery of copper was investigated and the optimum conditions were established The detection limit in two methods was 0.001 µg mL -1 . A pre-concentration factor was 400 for Mebqb- naphthalene absorbent and 200 for Mebqb-graphite absorbent. Adsorption capacity were 16.1 mg/g (copper/ Mebqb-graphite) and 2.6 mg/g (copper/ Mebqb- naphthalene). The relative standard deviation Mebqb- naphthalene absorbent for five independent determinations reached values of 2.0 and 2.3% for copper solutions of 0.1 and 5.0 µg mL -1 , respectively. The relative standard deviation Mebqb-graphite absorbent for three independent determinations reached values of 2.4% for copper solutions of 5.0 µg mL -1 . This procedure has been successfully applied to separate and determine the ultra trace levels of copper in the environmental samples, free from the interference of some diverse ions. Copper has been determined in river, tap and waste water samples, with recoveries of 92 to 105% with Mebqb-graphite as absorbent and 98 to 103% . with Mebqb-naphthalene as absorbent