The total amount of superoxide (O
2 -) and peroxide (O
2 2-) occluded in micropores of calcium aluminosilicate (Ca
12Al
10Si
4O
35; mayenite) was determined from their reaction with pulsed H
2. Mayenite was prepared by calcining precursor hydrogarnet, which was synthesized via hydrothermal reaction of a stoichiometric mixture of CaO, Al
2O
3, and amorphous SiO
2. Since a part of Ca
2+ in hydrogarnet could be substituted with other metal ions by adding a corresponding metal nitrate to the mixture, metal-substituted mayenite was also prepared by calcining the precursor metal-substituted hydrogarnet. Substitution of Ca
2+ with other metal ions markedly increased the amount of oxide anions reacting with pulsed H
2 and the amount was largest for Cu-mayenite. The amount of O
2 taken up in oxide anion-deficient mayenite was found to be largest for Cu-substituted mayenite. It was also confirmed that reaction between oxide anions in Cu-mayenite and pulsed H
2 and that between oxide anion-deficient Cu-mayenite and pulsed O
2 were completed even under a very high flow rate of the carrier gas, corresponding to the space velocity of >10
5 h
-1. A large amount of occluded oxide anions reacting with H
2 together with their quick regeneration in oxide anion-deficient mayenite leads us to expect that Cu-mayenite is applied as a new material with an excellent oxygen storage capacity to an automotive three-way catalyst.
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