EDTA is an important ligand used in many industrial products as well as in agriculture, where it is employed to
assist in phytoextraction procedures and the absorption of nutrients by plants. Due to its intensive use and recalcitrance,
it is now considered an emerging pollutant in water, so there is great interest in techniques suitable for
itsmonitoring. This work proposes amethod based on formation of the Mn(III)-EDTA complex after oxidation of
theMn(II)-EDTA complex by PbO2 immobilized on cyanoacrylate spheres. A design of experiments (DOE) based
on the Doehlert matrix was used to determine the optimum conditions of the method, and the influence of the
variables was evaluated using a multiple linear regression (MLR) model. The optimized method presented a linear
response in the range from 0.77 to 100.0 μmol L−1, with analytical sensitivity of 7.7 × 103 L mol−1, a coefficient
of determination of 0.999, and a limit of detection of 0.23 μmol L−1. Themethodwas applied using samples
fortified at different concentration levels, and the recoveries achieved were between 97.0 and 104.9%.