A simple and reliable method was developed for the determination ofserum copper and zinc in different chemical forms by graphite furnace atomicabsorption spectrometry (GFAAS) with ethanol-EDTA precipitation. The serum andethanol were mixed with volume ratio 1∶2. The mixture was incubated at 70 ℃ andultra-centrifuged to precipitate proteins. Zinc and copper can be released fromalbumin after EDTA treating. Thus, macroglobulin-zinc, ceruloplasmin-copper, andalbumin-bound zinc or copper could be determined by two proposed precipitationsteps. The determination limit of copper (3σ) was 1.2 μg?L-1 and the recoverywas 92.3%-104%, while the determination limit of zinc (3σ) was 0.098 μg?L-1,and the recovery was 90%-107%. This two-step precipitation method can be used todetermine serum zinc and copper in various chemical forms in tumor, Wilsonpatients and heathy human.