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The use of AC/DC magnetic susceptibility and impedance measurements to detect oxygen depletion effects in La
0.7Ca
0.3MnO
3±δ and NiMn
2O
4±δ spinel-type compounds is reported. For the NiMn
2O
4, for which no Mn
4+ was found, three superposed Debye relaxations were observed in the range 260–180
K. Otherwise, in La
0.7Ca
0.3MnO
3, the argon annealed has contributed to a decrease in
T
C, but the amount of Mn
4+ is still too high to allow the observation of a relaxation in this frequency window.