糠醛衍生-气相色谱/质谱法测定地表水中的肼和偏二甲基肼

摘要

建立了糠醛衍生-气相色谱/质谱法测定地表水中肼和偏二甲基肼两种肼类化合物的方法,优化了实验条件.在200mL水样(pH=7)中加入10mL0.05g/mL的糠醛衍生试剂,室温下反应2h,用15mL二氯甲烷萃取10min,氮吹至1.0mL后进样分析.本方法在0～100μg/L范围内线性良好,相关系数大于0.996.检出限分别为0.70μg/L和0.88μg/L;地表水加标样中肼和偏二甲基肼的RSD均小于21%(n=6);肼加标样品的回收率在71%～130%之间,偏二甲基肼加标样品的回收率在82%～124%之间.%The method to determine hydrazine and unsymmetrical dimethyl hydrazine in surface water by furfural derivation and GC/MS analysis was established.The analytical parameters were optimized.10-mL furfural derivation reagent was added into 200-mL sample (pH =7) at room temperature to react for two hours, and then the derivative product was extracted using 15-mL dichloromethane for 10 minutes.The sample was blown using nitrogen until becoming 1.0 mL volume for injection.This method had a good linearity in the range of 0 ～ 100 μg/L ( R ＞ 0.996).The detection limits of hydrazine and unsymmetrical dimethyl hydrazine were 0.70 and 0.88 μg/L, respectively.The RSDs of the spiked water samples for both hydrazine and unsymmetrical dimethyl hydrazine in surface water were less than 21％ (n = 6).The recoveries of the spiked samples of hydrazine and unsymmetrical dimethyl hydrazine were 71％ ～ 130％ and 82％ ～ 124％, respectively.