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丙酮衍生化-顶空-气相色谱法(NPD)测定水中水合肼

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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.
Study on the Determination of Hydrazine in Water by Acetone Derivatization-Headspace Gas Chromatography NPD
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 anti-interference ability,and can better meet the current monitoring requirements of hydrazine hydrate in drinking water sources.

hydrazine hydrate in wateracetone derivatizationheadspacegas chromatography

钟明霞、闫琨、徐小峰、冯晖、黄丽娟、李振宇

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云南省生态环境厅驻昆明市生态环境监测站,云南 昆明 650228

水中水合肼 丙酮衍生化 顶空 气相色谱(NPD)法

2024

中国环境监测
中国环境监测总站

中国环境监测

CSTPCD北大核心
影响因子:1.761
ISSN:1002-6002
年,卷(期):2024.40(6)