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    吹扫捕集-气相色谱-质谱法测定水体中1,3-丁二烯和1-溴丙烷的含量

    Determination of 1, 3-Butadiene and 1-Bromopropane in Water Body by Gas Chromatography-Mass Spectrometry with Purge-and-Trap

    • 摘要: 迅速采集地表水、工业废水或海水水样,使其充满样品瓶,在线加入内标氟苯,和样品同时在吹扫时间10 min、吹扫温度40 ℃、脱附温度180 ℃、脱附时间2 min条件下进行吹扫捕集,然后采用气相色谱-质谱法测定1,3-丁二烯和1-溴丙烷的含量。在色谱分析中,以DB-624色谱柱作固定相在升温程序下分离;在质谱分析中,以电子轰击离子源电离,选择离子监测模式检测。结果显示:1,3-丁二烯和1-溴丙烷的线性范围为1.0~40.0 µg·L−1,检出限(3.143s)分别为0.3,0.2 µg·L−1;对上述3种样品基质进行3个浓度水平的加标回收试验,回收率为81.4%~118%,测定值的相对标准偏差(n=6)为1.7%~12%。

       

      Abstract: The surface water, industrial wastewater, or seawater samples was rapidly collected by filling the sample bottles completely, and the internal standard fluorobenzene was added online. Both the samples and internal standard were simultaneously subjected to purge-and-trap analysis under the conditions of purge time of 10 min, purge temperature of 40 °C, desorption temperature of 180 °C, and desorption time of 2 min, and then 1,3-butadiene and 1-bromopropane were determined by gas chromatography-mass spectrometry. In the chromatographic analysis, separation was performed on DB-624 column as the stationary phase under temperature-programmed mode. In the mass spectrometric analysis, ionization was conducted by electron impact ion source, and detection was made in the selected ion monitoring mode. It was shown that linear ranges of 1,3-butadiene and 1-bromopropane were found in the range of 1.0-40.0 µg · L−1, with detection limits (3.143s) of 0.3, 0.2 µg · L−1, respectively. Spike recovery tests were made on the 3 aforementioned sample matrices at 3 concentration levels, giving recoveries in the range of 81.4%-118%, and RSDs (n=6) of the determined values ranged from 1.7% to 12%.

       

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