凌伟洁, 戎伟丰, 刘移民. 浸渍活性炭管采集溶剂解吸—气相色谱法测定空气中环氧乙烷[J]. 职业卫生与应急救援, 2015, 33(3): 193-197. DOI: 10.16369/j.oher.issn.1007-1326.2015.03.017
引用本文: 凌伟洁, 戎伟丰, 刘移民. 浸渍活性炭管采集溶剂解吸—气相色谱法测定空气中环氧乙烷[J]. 职业卫生与应急救援, 2015, 33(3): 193-197. DOI: 10.16369/j.oher.issn.1007-1326.2015.03.017
LING Weijie, RONG Weifeng, LIU Yimin. Determination of ethylene oxide by dissolved desorption-GC with sampling charcoal tube containing hydrobromic acid[J]. Occupational Health and Emergency Rescue, 2015, 33(3): 193-197. DOI: 10.16369/j.oher.issn.1007-1326.2015.03.017
Citation: LING Weijie, RONG Weifeng, LIU Yimin. Determination of ethylene oxide by dissolved desorption-GC with sampling charcoal tube containing hydrobromic acid[J]. Occupational Health and Emergency Rescue, 2015, 33(3): 193-197. DOI: 10.16369/j.oher.issn.1007-1326.2015.03.017

浸渍活性炭管采集溶剂解吸—气相色谱法测定空气中环氧乙烷

Determination of ethylene oxide by dissolved desorption-GC with sampling charcoal tube containing hydrobromic acid

  • 摘要: 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。

     

    Abstract: Objective New solid sorbent tubes were developed for capturing ethylene oxide (EO) in the air and the matched dissolved desorption-gas chromatography was established. Methods Based on the principle that EO could react with hydrobromic acid, the new solid sorbent tubes were developed, which were dipped with 5%(V/V) hydrobromic acid-methanol solution. The reaction product, generated in the process of capture,was desorbed with dimethylformamide, separated through capillary chromatographic column separation, and then detected by GC-ECD. Results The linear range of EO was 0.12-97.29 mg/L, and the related coefficients was 0.99997. The minimum quantification concentration was 0.01 mg/m3(sample volume was 3.0L).The average derivative efficiency was 95.67%-97.38%. The average desorption efficiency was 93.55%-98.49%. The intraday relative standard deviation (RSD) was 1.27%-1.96%, and the interday RSD was 2.49%-3.83%. The samples could be stored at room temperature for at least 6 days, and 8 days at 4 centigrade. Conclusion The new solid sorbent tubes containing hydrobromic acid were developed and could be applicable for collection of ethylene oxide (EO) in the air.

     

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