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《化学分析计量》 2019年第03期
DOI:10.3969/j.issn.1008-6145.2019.03.006
顶空气相色谱-质谱法快速测定废水中的α-甲基萘
曾珍,周姗,王奕奕,汪凌佳,陈峰
杭州市环境监测中心站,杭州 310007 
Rapid determination of α-methylnaphthalene in wastewater by headspace gas chromatography-mass spectrometry
ZENG Zhen, ZHOU Shan, WANG Yiyi, WANG Lingjia, CHEN Feng
Hangzhou Environmental Monitoring Center Station, Hangzhou 310007, China 
摘要:建立顶空气相色谱-质谱法测定废水中α-甲基萘的含量。优化色谱、质谱及顶空条件,选用DB-624 毛细管柱(30 m×0.32 mm,1.8 μm),在柱流量1.5 mL/min 条件下采用电子轰击电离源,全扫描定性,选择离子外标法定量。α-甲基萘的质量浓度在40~1 500 g/L 范围内与其色谱峰面积呈良好的线性关系,相关系数大于0.999 5,当废水取样量为10.0 mL 时,方法检出限为4.8 μg/L。在3 个不同加标水平下,实际废水样品中α-甲基萘的平均回收率为89.8%~97.6%,测定结果的相对标准偏差为1.5%~7.1%(n=6)。该方法快速灵敏、准确度高、重现性好,适用于废水样品中α-甲基萘的应急监测。 
Abstract:A method was established to determine α-methylnaphthalene in wastewater by headspace gas chromatography-mass spectrometry. The analytical conditions of headspace and chromatography-mass spectrometry were optimized. The analysis was carried out with a capillary column DB-624(30 m×0.32 mm, 1.8 μm) under electron ionization conditions at flow rate of 1.5 mL/min, the qualitation was performed by the mode of scanning and the quantitation was performed by the external standard method using selected ion. The mass concentration of α-methylnaphthalene had good linear relationship with the chromatographic peak area in the range of 40-1 500 g/L, and the correlation coefficient was more than 0.999 5. The detection limit was 4.8 μg/L as using 10.0 mL wastewater samples. The average recoveries of α-methylnaphthalene in wastewater samples were 89.8%-97.6% at three different addition levels, and the relative standard deviations of determination results were 1.5%-7.1%(n=6). The method is rapid, sensitive, accurate and reproducible, and it is suitable for the determination of α-methylnaphthalene in wastewater samples for emergency monitoring. 
关键词:α-甲基萘;气相色谱-质谱法;顶空;废水 
Keywords:α-methylnaphthalene; gas chromatography-mass spectrometry; headspace; wastewater 
基金:杭州市农业和社会发展科研项目(20191203B66) ;杭州市环境保护科研课题(2010013) 
本文引用格式:
曾珍,周姗,王奕奕,等. 顶空气相色谱- 质谱法快速测定废水中的α- 甲基萘[J]. 化学分析计量,2019,28(3):21-24.
ZENG Z,ZHOU S,WANG Y Y,et al. Rapid determination of α-methylnaphthalene in wastewater by headspace gas chromatography-mass spectrometry[J]. Chemical analysis and meterage,2019,28(3):21-24. 

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