丙酮衍生化-顶空-气相色谱法(NPD)测定水中水合肼  

Study on the Determination of Hydrazine in Water by Acetone Derivatization-Headspace Gas Chromatography NPD

作　　者：钟明霞 闫琨 徐小峰 冯晖 黄丽娟 李振宇 ZHONG Mingxia;YAN Kun;XU Xiaofeng;FENG Hui;HUANG Lijuan;LI Zhenyu(Yunnan Provincial Department of Ecology and Environment in Kunming Ecological Environmental Monitoring Station,Kunming 650228,China)

机构地区：[1]云南省生态环境厅驻昆明市生态环境监测站,云南昆明650228

出　　处：《中国环境监测》2024年第6期197-203,共7页Environmental Monitoring in China

摘　　要：建立了丙酮衍生化-顶空-气相色谱法(氮磷检测器)测定水中水合肼的新方法。水中水合肼在弱碱性或碱性环境下,与丙酮发生衍生化反应,经顶空前处理,气相色谱分离后,用氮磷检测器检测。优化了此方法在测定水中水合肼时的衍生化反应条件、盐析效应、顶空温度、顶空平衡时间和反应体系的酸碱性等实验条件。实验结果表明:使用该方法测水合肼,校准曲线线性好(浓度范围为0.020~1.00 mg/L),相关系数为0.9997,水合肼检出限为0.004 mg/L(折合以肼计为0.0025 mg/L),方法重现性和准确度好,RSD为2.7%~5.8%,加标回收率为89.6%~105%。与传统的分光光度法相比,该方法具有简便、快速、抗干扰能力强等特点,能较好满足现阶段饮用水源地水体中水合肼的监测要求。A method for the determination of hydrazine hydrate in water by acetone derivatization and headspace gas chromatography(NPD)was established.Hydrazine hydrate in water was derivated with acetone in a weakly alkaline or alkaline environment and treated by headspace,then separated by gas chromatography and detected by nitrogen and phosphorus detector(NPD).In this paper,the derivatization reaction conditions,salting-out effect,headspace temperature,headspace equilibrium time and acidity-alkalinity of reaction system were deeply researched.The results showed that the method had good linearity in the range of 0.020-1.00 mg/L(r=0.9997),and the detection limit of hydrazine hydrate was 0.004 mg/L(convert into 0.0025 mg/L by hydrazine).The method's repeatability and accuracy were good,RSD were 2.7%-5.8%and the recoveries were 89.6%-105%.Compared with the traditional spectrophotometry,the method has the characteristics of simple,rapid and strong antiinterference ability,and can better meet the current monitoring requirements of hydrazine hydrate in drinking water sources.

关 键 词：水中水合肼 丙酮衍生化 顶空 气相色谱(NPD)法 

分 类 号：X832[环境科学与工程—环境工程]