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A sudden leak of phenylamine is an urgent environmental issue due to its liquidity and volatility. To overcome this difficulty, the decontamination efficiency of spray, foam, and activated carbon to phenylamine was explored using simulated leak box. Furthermore, a new decontamination method of foam coupling with acidic spray was proposed to decontaminate phenylamine. Its decontamination efficiency for phenylamine gas was up to 90% after 3 min adsorption at 3:1 mass ratio and phenylamine liquid was solidified quickly.