职业环境中肼的毛细管气相色谱分析
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O657

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重庆市基础科学与前沿技术研究项目(CSTC2017jcyjAX0446);重庆医药高等专科学校校级课题(ygz2018308)。


Analysis of hydrazine in occupational environment by capillary gas chromatography
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    摘要:

    用过量的糠醛衍生转化肼,用质谱对肼的糠醛衍生晶体进行结构定性,对肼糠醛衍生物的晶体、溶剂及肼糠醛衍生物的提取液进行毛细管气相色谱对比分析,获得可靠的定性定量分析信息,优化衍生、萃取和色谱分析等条件,用标准曲线、精密度和准确度试验进行方法评价。实验表明,在糠醛过量的条件下,肼完全转化为2糠醛嗪,保留时间为6.20 min,方法检出下限为0.007 8 mg/L,相对标准偏差2.5%,加标回收率98%~100%。方法的色谱峰形对称、准确、灵敏度高、选择性好,为不同实验室仪器及色谱柱条件下分析检测肼提供了一种快速、准确的条件探索程序。

    Abstract:

    Hydrazine is derived with excessive furfural. The crystal of hydrazine derivative conversion is characterized by mass spectrometry. The comparative analyses are made between the hydrazine-derived furfural crystal, solvent, as well as extraction solution of furfural derivatives of hydrazine by the method of capillary gas chromatography. Reliable qualitative and quantitative analytical information is obtained, and the conditions of derivation, extraction and chromatographic analysis are optimized. The method is evaluated by standard curve, precision and accuracy tests. Experiments show that in the case of excessive furfural, hydrazine is completely converted to 2-furaldehyde azine, whose retention time is 6.20 min. The detection limit of the method is 0.007 8 mg/L, the relative standard deviation is 2.5%, and the recovery is in the range of 98% to 100%. The method has the advantages of symmetrical peak shape, high accuracy, high sensitivity and good selectivity. It provides a rapid and accurate procedure for the analysis and determination of hydrazine under different laboratory instruments and chromatographic column conditions.

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林一民,周彬,汤利娜,王丽娟,张稳稳,季卫刚,杨旭.职业环境中肼的毛细管气相色谱分析[J].重庆大学学报,2019,42(12):60-66.

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  • 收稿日期:2019-07-10
  • 在线发布日期: 2019-11-21
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