优化顶空-气相色谱/质谱联用法测定水中苯系物
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中国科学院南京土壤研究所所基金支撑课题(20752010028)资助


Optimized determination of BTEXs in water samples with headspace-gas chromatography/mass spectrometer
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    摘要:

    采用VF-5ms和CP-8ms毛细管色谱柱、顶空-气相色谱/质谱联用法测定水中的苯系物,并对实验条件,尤其是顶空条件进行了优化。结果表明,含有水样的10 ml顶空瓶在加热阱以500 r min-1振摇20 s,停90 s,液气比为6:4,加盐(NaCl)量为0.4 g ml-1,于60 ℃时平衡30 min,即可达到顶空的最佳实验结果;且本方法的仪器精密度为1.41%~6.52%,检出限为0.10~0.13 μg L-1不等,实验得出各目标物的标准曲线线性相关性均为r≥0.999,加标样品回收率为98.4%~100.2%,完全符合有机分析的要求。

    Abstract:

    BTEXs in water samples were determined with VF-5 ms and CP-8ms capillary-column and Headspace-Gas Chromatography/Mass spectrometer (HS-GC/MS) under modified conditions, especially with the headspace. Results show that when 10 ml flasks with water sample accounting for 60% of each flask in volume were agitated for 20 sec. at a rate of 500 r min -1, in the heated shaker, then kept still for 90 sec. mixed with 2.4 g NaCl in each flask and left for equilibrium for 30 min. under 60 ℃, optimal results could be obtained. The BTEXs detection limits of the method varied the range of 0.10~0.13 μg L -1; the standard curve correlation coefficient (r) of each BTEXs target was more than or equal to 0.999; and the sample recovery rate lingered in the rang of 98.4%~100.2% with precision being 1.41%~6.52% (n=7). All demonstrate that the method meets the requirements of organic analysis.

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陈 虹,韩 勇,王 曦,钟 明,靳 伟.优化顶空-气相色谱/质谱联用法测定水中苯系物[J].土壤学报,2013,50(5):992-997. DOI:10.11766/trxb201301150030 Chen Hong, Han Yong, Wang Xi, Zhong Ming, Jin Wei. Optimized determination of BTEXs in water samples with headspace-gas chromatography/mass spectrometer[J]. Acta Pedologica Sinica,2013,50(5):992-997.

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  • 收稿日期:2013-01-15
  • 最后修改日期:2013-04-09
  • 录用日期:2013-04-16
  • 在线发布日期: 2013-07-03
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