高效液相色谱法测定水中痕量偏二甲肼  

Determination of trace unsymmetrical dimethylhydrazine in water by high performance liquid chromatography

作　　者：韩莹[1,2] 陈忠林[1,2] 沈吉敏[1,2] 杨磊[2] 刘宇[1,2] 

机构地区：[1]哈尔滨工业大学城市水资源与水环境国家重点实验室,哈尔滨150090 [2]哈尔滨工业大学市政环境工程学院,哈尔滨150090

出　　处：《哈尔滨工业大学学报》2013年第8期34-38,共5页Journal of Harbin Institute of Technology

基　　金：国家自然科学基金资助项目(50578052;51078105);城市水资源与水环境国家重点实验室自主课题(2010DX12)

摘　　要：为了快速、准确地测定水中痕量偏二甲肼(UDMH),通过比较不同检测波长、流动相种类及比例下的检测效果优化色谱条件,同时通过比较不同衍生时间、溶液pH、衍生剂用量下的检测效果优化衍生条件,建立了高效液相色谱测定UDMH的方法.优化得到的色谱条件为:采用C18柱和紫外检测器进行分离和检测,选定390 nm作为检测波长,以乙腈与水为流动相且V(乙腈)∶V(水)=4∶1.优化得到的衍生条件为:水样以4-硝基苯甲醛(在总体积中的浓度为3 mmol/L)为衍生剂,溶液pH保持为5.5,75℃水浴15 min.在优化的条件下进行检测,衍生物的保留时间为2.64 min,峰面积(峰高)对UDMH质量浓度的相关系数≥0.999 4,检出限为0.5μg/L,对模拟水样检测的相对标准偏差≤1.69%,加标回收率为95.7%～102.7%.该方法检测快速,具有良好的线性关系,检出限低,精密度和准确度高,适合测定水中痕量的偏二甲肼.For the fast and accurate determination of trace unsymmetrical dimethylhydrazine（UDMH）,a high performance liquid chromatography method was developed after the optimization of the chromatographic conditions by comparing the detection results under the different detection wavelengths,types and proportions of the mobile phase and the optimization of the derivative conditions by comparing the detection results under the different derivative time,the solution pH values and the dosages of derivatizing regents.The optimized conditions are as following,for the chromatography： separation by the C18 column and detection by the ultraviolet detector,390 nm as the wavelength,the acetonitrile and water with a volume ratio of 4：1 were taken as the mobile phases;for the derivatization： derivatization with 4-nitrobenzaldehyde（the molar concentration is 3 mmol/L in the total volume）,the solution pH 5.5,heating in a water bath at 75 ℃ for 15 min.The results showed that under the optimized conditions,the retention time of the derivative product was 2.64 min,the correlation coefficients of peak area（peak height） to mass concentration was equal to or more than 0.999 4,the detection limit was 0.5 μg/L.For the simulated water sample,the relative standard deviation was equal to or less than 1.69%,and the recovery of standard addition was 95.7%-102.7%.The method is rapid in determination,and has good linear relationship,a low detection limit,the precision and accuracy for determining trace UDMH in water.

关 键 词：偏二甲肼 高效液相色谱 衍生化 痕量分析 4-硝基苯甲醛 

分 类 号：X703.1[环境科学与工程—环境工程]