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2-(pyridine-2-yl)-N-p-chlorohydrazinecarbothioamide (HCPTS) was synthesized, characterized and successfully applied for the preconcentration of Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II) in water, blood, and urine samples prior to graphite furnace atomic absorption determination (GFAAS); Hg was determined by cold vapor technique. Under the optimum experimental conditions (i.e. pH = 8, 10–4 M of HCPTS, 0.05% w/v of Triton X-114), calibration graphs were linear in the range of 0.02 to 200 ng?mL–1 for Co(II), Cd(II), Pb(II) and Ni(II); 0.03 to 200 ng?mL–1 for Cu(II); 0.07 to 200 ng?mL–1 for Fe(II) and Zn(II) and 0.02 to 150 ng?mL–1 for Hg(II). The enrichment factors were 43, 51, 41, 46, 54, 40, 45 and 52 for Cu(II), Ni(II),Zn (II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The limit of detection were found to be 0.019, 0.094, 0.0514, 0.052, 0.0165, 0.047, 0.068 and 0.041 ng?mL–1 for Cu(II), Ni(II), Zn(II), Cd(II), Co(II), Pb(II), Fe(II), and Hg(II), respectively. The developed method was applied to the determination of these metal ions in water, blood and urine samples with satisfactory results.