五氟苯甲酰氯衍生-气相色谱-质谱法测定地表水中一甲基肼  

Determination of Mono-methyl Hydrazine by Pentafluorobenzoyl Chloride Derivatization and Gas Chromatography-Mass spectrometry(GC-MS) in Surface Water

作　　者：张渝[1,2] 程小艳[1] 钱蜀 王利[2] 

机构地区：[1]四川省环境监测中心站,四川成都610041 [2]四川大学制革清洁技术国家工程实验室,四川成都610065

出　　处：《中国环境监测》2012年第3期86-89,共4页Environmental Monitoring in China

基　　金：四川省环境保护科技项目计划(2008HBB006)

摘　　要：建立了五氟苯甲酰氯衍生-气相色谱-质谱法测定地表水中一甲基肼的方法。取200ml水样,调节后的pH为10,加入20ml衍生剂,在室温下剧烈振荡衍生1h,40ml二氯甲烷萃取10min,浓缩至1.0ml后用气相色谱-质谱联用分析。方法在5～500μg/L浓度范围内线性良好,相关系数大于0.996,方法检出限为2.67μg/L;加标水样的相对标准偏差为9.54%和8.38%;加标水样回收率为79.08%～102.96%。The method was established to determine the methylhydrazine by pentafluorobenzoyl chloride derivatization in surface water coupled with gas chromatography-mass spectrometry.The volume of water sample was 200ml,the adjusted value of pH was 10,the amount of derivative reagents was 20ml,the time of derivatization was 1h,the way of derivatization was shaking violently.After derivatization ending,the derivatization solution was extracted 10min by 40ml dichloromethane.After extraction solution was concentrated to 1ml,gas chromatography-mass spectrometry was used for quantitative and confirmatory analysis of the derivative product.The method linearity range was 5~500μg/L.The correlation coefficient was not less than 0.996.The detect limit of the method was 2.67μg/L.The RSD of the spiked samples were 9.54% and 8.38%,respectively.The recovery of the spiked samples was 79.08%~102.96%.

关 键 词：衍生 甲基肼 气相色谱-质谱联用 地表水 

分 类 号：X830.2[环境科学与工程—环境工程]