便携式顶空-气相色谱质谱联用仪测定土壤中四氢噻吩
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O65;X833

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北京市劳动保护科学研究所2021年改革与发展项目(k120-5)和国家重点研发计划项目(2019YFE0194500)资助。


Determination of Tetrahydrothiophene in Soil with Portable Headspace-gas Chromatography-mass Spectrometry
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The National Key Research and Development Program of China (No. 2019YFE0194500)

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    摘要:

    四氢噻吩常用作燃气的气味添加剂,用以追踪燃气的泄露。为建立一套便携式顶空-气相色谱质谱联用法(HS-GC/MS)检测土壤中四氢噻吩的浓度,采用正交试验对顶空进样条件(平衡温度、平衡时间和进样压力)和气相色谱质谱检测条件进行了优化。结果表明:顶空进样的最佳条件为平衡温度80℃,平衡时间20 min,进样压力100 kPa;便携式气相色谱质谱联用法(GC/MS)的升温程序为:初始柱温60℃,保持2 min,以10℃/min的速率升至90℃,保持4 min,然后以20℃/min的速率升至200℃,保持10 min。在最佳条件下,方法的检出范围为0.005~10.000 mg/kg,不同浓度四氢噻吩的加标回收率为82.4%~98.5%,日内和日间精密度相对标准偏差为4.6%~7.5%,所建方法快速高效、重复性好,可用于土壤中四氢噻吩现场快速检测。

    Abstract:

    Tetrahydrothiophene is commonly used as an odor additive in combustible gas to track of gas leaks. In order to develop a method by using portable headspace gas chromatography with mass spectrometry (HS-GC/MS) to determine tetrahydrothiophene in soil, orthogonal test was adopted to optimize the parameters of headspace injection, including different equilibrium temperature and time, different injection pressure and different GC/MS detection parameters. Results showed that:1) The optimal conditions for headspace injection were equilibrium temperature 80℃, equilibrium time 20 min, and injection pressure 100 kPa. 2) The heating procedure of the portable GC/MS as follows:the initial column temperature was 60℃, kept for 2 min, then raised up to 90℃ at 10℃/min, kept for 4 min, and to 200℃ at a rate of 20℃/min, kept for 10 min. 3) Under such conditions, the detection range for this method of tetrahydrothiophene concentration was between 0.005 mg/kg and 10.000 mg/kg, recovery rate between 82.4%-98.5%, intraday and intraday precision relative standard deviation between 4.6%-7.5%. The established method is fast, efficient and repeatable, and can be used to on-site detect tetrahydrothiophene in soil.

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舒木水,贺佳欣,淡默,尤雅楠,丁玎,王昱,周芃垚,姚伟,纪晓慧.便携式顶空-气相色谱质谱联用仪测定土壤中四氢噻吩[J].土壤,2021,53(5):1095-1100. SHU Mushui, HE Jiaxin, DAN Mo, YOU Yanan, DING Ding, WANG Yu, ZHOU Pengyao, YAO Wei, JI Xiaohui. Determination of Tetrahydrothiophene in Soil with Portable Headspace-gas Chromatography-mass Spectrometry[J]. Soils,2021,53(5):1095-1100

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