采用水蒸气蒸馏、二氯甲烷萃取及氮气吹扫浓缩等样品预处理方法,建立了含偏二甲肼污水中N-亚硝基二甲胺(NDMA)的气相色谱-质谱(GC-MS)分析方法.以N-亚硝基二甲胺的浓度在0.31~1.54 mg·L-1范围内对峰面积做校准曲线,回归方程Y=2.60×104x-4.49×103(r=0.999 5),于100 mL蒸馏水(即空白溶液)中分别加入2.016 μg及10.08 μg NDMA,按方法测定并计算回收率及标准偏差,测定结果的相对标准偏差为4.82%和4.96%,回收率为88.8%和89.3%,检出限(S/N=3)为2 μg·L-1.

Hyphenation of gas chromatography and mass spectrometry was applied to the determination of N-nitrosodimethylamine (NDMA),a probable degradation compound of 1,1-dimethyl hydrazine,in 1,1-dimethylhydrazine containing waste water,using selected ion monitoring mode. The waste water sample was pretreated by steam distillation,extraction with dichloromethane and concentration by blowing with nitrogen. Linear relationship between the peak area and concentration of NDMA was obtained in the range of 0.31-1.54 mg·L-1,corresponding to the linear regression equation Y=2.60×104 x-4.49×103 (r=0.999 5),with detection limit (S/N=3) of 2 μg·L-1. Tests for recovery and precision of this method were made by adding 2.016 μg and 10.08 μg of NDMA to 100 mL of distilled water (i.e. blank solution),and determined by the proposed method,the results of recovery obtained were 88.8% and 89.3%,results of RSD′s found were 4.82% and 4.96% respectively.