An optimised electrochemical technique, linear sweep voltammetry (LSV) in KOH solution (LSV-KOH) was confronted with the double loop electrochemical Potentiokinetic reactivation (DL-EPR) to verify which is the best technique to quantify deleterious phases (DP) in a UNS S32750 super duplex stainless steel. DL-EPR presented an error in determination of deleterious phases in the range of 6.9-100%. LSV-KOH show a better accuracy in quantification of deleterious phases volume fractions, the error range for LSV-KOH was 2.4-26.2%. When the morphology of sigma changes from lamellar to divorced, was observed modifications on LSV-KOH voltammograms. In specimens where lamellar morphology is present, the voltammograms show two peaks curve. Meanwhile, in specimens where occurred also divorced precipitation of sigma the voltammograms changes to a 3 peaks curve. This feature is due to the dissolution of sigma phase boundaries which has different compositions according to the form of sigma precipitation.

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