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目的研制用于捕集空气中环氧乙烷(EO)的固体吸附剂管,并建立配套的气相色谱法。方法基于EO能与氢溴酸发生开环反应生成2-溴乙醇的原理,采用研制的固体吸附剂管捕集空气中EO,在捕集过程中反应生成2-溴乙醇,经二甲基甲酰胺解吸、毛细管色谱柱分离后,运用电子俘获检测器对其进行检测。结果在0.12~97.29 mg/L范围内,EO质量浓度与实验测得峰面积呈线性关系,相关系数为0.999 97;批内精密度相对标准偏差(RSD)为1.27%~1.96%,批间精密度RSD为2.49%~3.83%;平均解吸效率为93.55%~98.49%;平均衍生效率为95.67%~97.38%;定量下限为0.03 mg/L;最低定量质量浓度为0.01 mg/m3(以采集3.0 L空气计)。样品在室温下可保存6 d,在4℃冰箱中至少可保存8 d,这比国家标准方法需要当天尽快测定这一要求有了明显改进。结论研制的固体吸附剂管及其配套的测定方法适合于空气中EO的采样以及检测。
Objective To develop a solid sorbent tube for the capture of ethylene oxide (EO) in air and to establish a gas chromatograph. Methods Based on the principle that EO can react with hydrobromic acid to produce 2-bromoethanol, EO in the air was captured by the developed solid sorbent tube and reacted with 2-bromoethanol in the process of catalysis. Amide desorption, capillary column separation, the use of electron capture detector to detect it. Results In the range of 0.12 ~ 97.29 mg / L, the linear relationship between the mass concentration of EO and the measured peak area was obtained. The correlation coefficient was 0.999 97. The relative standard deviation (RSD) of in-batch precision was 1.27% ~ 1.96% The average RSD was 2.49% -3.83%; the average desorption efficiency was 93.55% ~ 98.49%; the average derivatization efficiency was 95.67% ~ 97.38%; the lower limit of quantitation was 0.03 mg / L; the lowest concentration was 0.01 mg / L air meter). The sample can be stored for 6 days at room temperature and at least 8 days in a refrigerator at 4 ° C. This is a significant improvement over the requirement of the national standard method for quickly determining the same day. Conclusion The developed solid sorbent tubes and their supporting determination methods are suitable for the sampling and detection of EO in the air.