衍生化-气相色谱法测定密闭环境空气中偏二甲肼  

Determination of Unsymmetrical Dimethylhydrazine in Air of Closed Environment with Gas Chromatography after Derivatization

作　　者：韦桂欢[1] 龙庆云[1] 杨品[1] 王晓利[1] 陈巍[1] 

机构地区：[1]中国船舶重工集团公司第七一八研究所,河北邯郸056027

出　　处：《舰船防化》2015年第1期17-21,共5页

摘　　要：建立了气相色谱法测定密闭环境空气中偏二甲肼的检测方法。空气中的偏二甲肼经涂有硫酸的硅胶采样管富集采样，采集后的硅胶经0．2mol·L-1。硫酸溶液解吸30min，以糠醛／乙酸钠溶液作为衍生化试剂在30℃水浴中进行衍生30min，最后用乙酸乙酯萃取10min，得到的萃取液样品以弱极性毛细管色谱柱分离，气相色谱一氢火焰检测器检测偏二甲肼衍生物，从而间接测定偏二甲肼的含量。实验讨论了不同极性色谱柱对样品分离的效果，优化了样品解吸时间、衍生化时间、衍生化温度对测定结果的影响。方法线性曲线相关系数为0．9991，回收率在86．2％～95．O％，相对标准偏差在6．13％～11．97%，检出限为0．005mg·m-3。该方法操作简便，选择性好，回收率较高，可满足密闭环境空气实际检测需要。In this report, the methods for determinating unsymmetrical dimethylhydrazine in air of closed environment with gas chromatography were researched. Unsymmetrical dimethylhydrazine in air were collected with silicon tube, then desorbed by 0.2 tool /L H2SO4 for 30 minutes, derivatized with furaldehyde / sodium acetate solution in 30 ~C water bath for 30 minutes. The sample solution was extracted with acetic ether for 10 min. After extraction, the sample solution was carried out by gas chromatography with flame ionization detector on the weak polar capillary column of DB-5. The conditions of different polar capillary column, the influences of different desorption time, derivative time and derivative temperature on the determined result, were optimized. The coefficient of correlation for the calibration curve was 0.9991, the recoveries varied from 86.2% to 95.0%, the relative standard deviations were between 6.13% and 11.97% and the detection limit was 0.005mg.m-3. The established method was simple and of high selectivity, high recoveries, and could meet the practical testing requirements.

关 键 词：密闭环境 空气 偏二甲肼 测定 气相色谱法 

分 类 号：O659.21[理学—分析化学]