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In a suitable pH buffer solutions, sodium diethyldithiocarbamate (DDTC) reacts with some divalence metal ions M(II) to form (M-DDTC)( n ) chelate complex nanoparticles, which exhibit different luminescence properties. There is a strongest luminescence peak at 470 nm for the Co(II)-DDTC system, three peaks at 330, 470, and 630 nm for the Cu(II)-DDTC system, three peaks at 420, 470, and 630 nm for the Cd(II)-DDTC system, four peaks at 350, 400, 435, and 470 nm for the Ni(II)-DDTC system, two peaks at 408 and 470 nm for the Pb(II)-DDTC system, two peaks at 415 and 470 nm for the Fe(II)-DDTC system. The different luminescence properties of (M-DDTC)( n ) chelate complex nanoparticles was explained. Under the optimal conditions, the luminescence intensity of (Co-DDTC)( n ) chelate complex nanoparticles at 470 nm (F (470 nm)) is linear to Co(II) concentration in the range of 0.012-1.44 microg/mL. The detection limit is 0.0023 microg/mL. A novel luminescence method has been proposed for the determination of cobalt in Vitamin B(12) samples, with satisfactory results.