The catalytic activity of a new catalyst for NO reduction is usually obtained by a gas-solid phase experiment. For the first time, a relationship has been established between catalytic performance and electrochemistry property. A bimetallic catalyst showed a low-temperature activity and removed 67.27% of NO at 300 °C, 33.39% bigger than a single-metallic catalyst. The bimetallic catalyst removed 9.770 mmol/g of NO after 1440 min, 5.212 mmol/g bigger than the single-metallic one. At the same time, the bimetallic catalyst showed a reduction capacity of 0.441 mmole/g. In comparison, the single-metallic one only had 0.242 mmole/g. Moreover, the limiting current of bimetallic catalyst (4.020 eA) was also bigger than that of single-metallic one (3.698 eA). Therefore, a catalyst for NO reduction showed better catalytic activity and electron-transfer ability at the same time. In other words, the catalytic activity of a catalyst can be potentially estimated by detecting its electrochemistry properties.