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The electrochemical preparation of Te 2− and Se 2− ions was carried out in NaOH aqueous solution, with high yield and good stability, and applied in the preparation of negatively charged CdTe and CdSe quantum dots (QDs). A CdCl 2 aqueous solution containing thioglycolic acid (TGA) stabilizer was mixed with the electrochemically generated Te 2− or Se 2− ions in a quite reproducible and clean one pot process, without the use of chemical reducing agents. The CdTe and CdSe QDs had good stability and high luminescence with an average size of d = 3.9 nm and 2.6 nm, respectively, the quantum yields and lifetimes were also determined. Hg 2+ was efficiently quantified in the presence of the synthesized TGAcapped CdTe and CdSe, making possible the application of these QDs as chemical sensors.