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A sequential AdSV method based on the accumulation of Zr(IV) and V(V) as cupferron‐oxalic acid‐1,3‐diphenylguanidine (COD) complexes at the HMDE was used to determine traces of these metals in samples with different ionic strengths. DP mode, Eads −0.6 and −0.2 V (vs. Ag/AgCl, 3 mol L−1 KCl), tads 400 and 20 s and 10 and 60 mV s−1 scan rates were used for Zr(IV) and V(V), respectively. Epeak were −0.95 (Zr(IV)‐COD) and −0.65 V(V(V)‐COD). The methodology was applied in samples of rivers, estuaries (in Germany and Brazil) and coastal and open seawater.
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