Abstract: The qualitative and quantitative analysis of hydrogen and carbon monoxide produced by radiation degradation of N,N-diethyl hydroxylamine is performed on a 2 m column packed with 5? (molecular) sieve and equipped with a thermal conductivity detector. The analysis of hydrogen employs argon as a carrier gas, the column temperature is 85 ℃ and the detector temperature is 110 ℃;the (analysis) of carbon monoxide employs hydrogen as a carrier gas,the column temperature is 50 ℃ and the detector temperature is 80 ℃. The results show that the volume fraction of hydrogen is increased with the increase of dose,but has little relationship with the concentration of N,N-diethyl hydroxylamine. Carbon monoxide is only produced when the absorption dose is very high and the volume fraction is very (low).