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 |
投稿时间:2023-06-14 修订日期:2023-09-20 |
DOI:10.19316/j.issn.1002-6002.2024.06.20 |
中文关键词: 水中水合肼 丙酮衍生化 顶空 气相色谱(NPD)法 |
英文关键词:hydrazine hydrate in water acetone derivatization headspace gas chromatography |
基金项目: |
|
通讯作者:冯晖* 云南省生态环境厅驻昆明市生态环境监测站, 云南 昆明 650228 |
摘要点击次数: 276 |
全文下载次数: 82 |
中文摘要: |
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0.999 7,水合肼检出限为0.004 mg/L (折合以肼计为0.002 5 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。 |
英文摘要: |
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. |
查看全文 查看/发表评论 下载PDF阅读器 |
|
|
|