化工废水中N-亚硝基二正丙胺的吹扫捕集-GC-MS测定法  

Determination of Nitrosodipropylamine in Chemical Industrial Wastewater by Gas Chromatography-Mass Spec-troscopy Coupled With the Purge and Trap Method

作　　者：钟鸣文[1] 盛华栋 金明娟[1] 计时华[1] 

机构地区：[1]浙江大学医学院,浙江杭州310031 [2]浙江省技术检督局,浙江杭州310007

出　　处：《环境与健康杂志》2003年第3期179-180,共2页Journal of Environment and Health

摘　　要：目的建立简单快速提取并测定N-亚硝基二正丙胺(NDPA)的方法。方法采用Trap3捕集管,利用标准吹扫捕集程序(吹扫气体流速40ml/min,吹扫时间11min,解吸温度225℃,解吸时间4min,烘烤温度230℃,烘烤时间10min),有效富集了化工废水中μg/L级的NDPA,建立了吹扫捕集(P&T)气相色谱质谱联用(GC-MS)化学源(CI)选择离子模式(uSIS)快速、准确分析废水中NDPA的分析方法。结果方法的相对标准偏差为7.5%;废水的加标回收率在62.60%～96.31%;在5～30μg/L范围内线性良好,线性回归系数为0.978;方法的最低检出限为3μg/L。结论采用P&T-GC-MS/CI/uSIS法可用于化工废水中半挥发性有机物NDPA的测定。Objective To establish a method for the simple and rapid extraction and detection of nitrosodipropulamine(NDPA).Methods NDPA at levels ofμg /L grade in chemical industrial wastewater was enriched efficiently using the purge and trap(P&T)method with a Trap3tube under the standard program,including the flow rate of purge gas(40ml/min),the time of purge(11min),the temperature of desorb(225℃),the time of desorb(4min),the temperature of bake(230℃)and the time of bake(10min).The NDPA concentrations were determined by gas chromatography-mass spectroscopy(GC-MS )and chemical ionization(CI )and select ion mode(uSIS)coupled with the purge and trap(P&T)(P&T/GC-MS/CI /uSIS)method Results The detection limit,recovery rates and relative standard deviation(RSD)of the method were3μg /L,62.60%-96.31%and7.5%respectively.The linearity of method was good in the5-30μg /L range with the correlation coefficient 0.978.Conclusion The P&T/GC-MS/CI /uSIS method could be used to detect semi-volatile NDPA in chemical industrial wastewater.

关 键 词：吹扫捕集 GC-MS N-亚硝基二正丙胺 废水 化工 

分 类 号：R123.1[医药卫生—环境卫生学] O657.7[医药卫生—公共卫生与预防医学]