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Mg–Al–Zn alloys with different Al content and different cooling conditions were prepared. The solid solution content of Al and Zn in the alloy was determined by electrochemical phase separation. The results show that Al has a large amount of solid solution, while Zn has a very low amount. Al can play a role in solid solution strengthening, while Zn is very small. Al has a repulsive effect on Zn and reduces the solid solubility of Zn. The higher the Al content it has, the larger the Al solid solution and the smaller the Zn solid solution we observe. The higher the solidification cooling rate is, the greater the solid solution amount of Al and Zn is.