Abstract: This paper reports the gas chromatographic analysis of gas hydrocarbons possibly produced by the radiation degradation of N,N-dimethylhydroxylamine and N,N-diethylhydroxylamine, porous layer open tubular column coated with aluminum oxide and flame-ionization detector are used. The best gas chromatographic analysis condition is as follow: column temperature: two steps programmed temperature: first step: initial temperature: 40 ℃, initial isothermal period: 9 min, programmed heating rate: 6 ℃/min, final temperature: 88 ℃, final isothermal period: 1 min; second step: initial temperature: 88 ℃, initial isothermal period: 1 min, programmed heating rate: 3 ℃/min, final temperature: 200 ℃, final isothermal period: 1 min; detector temperature: 250 ℃.