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目的建立同时检测工作场所空气中环氧乙烷(EO)、环氧丙烷(PO)和环氧氯丙烷(ECH)的气相色谱测定方法。方法样品采用活性炭管采集,5%(V/V)甲醇-二氯甲烷溶液解吸,经毛细管色谱柱分离,氢火焰离子化检测器测定。结果本方法 EO、PO和ECH质量浓度分别在0.24~960.00、0.60~2 384.00、0.12~472.40 mg/L线性关系良好,相关系数为0.999 95~0.999 96;最低检出浓度分别为0.06、0.04和0.02 mg/m3,最低定量浓度分别为0.16、0.13、0.07 mg/m3(以采集1.5 L空气计);平均解吸效率分别为79.21%~89.74%、86.06%~93.38%、90.77%~95.53%;方法批内精密度分别为2.52%~3.68%、1.64%~3.09%、2.15%~3.53%,批间精密度分别为2.69%~4.21%、1.87%~3.39%、3.69%~4.54%。EO、PO和ECH样品在-20℃冰箱中分别至少可保存5、7、7 d。结论本方法灵敏度高,精密度好,操作简单,适用于工作场所空气中EO、PO和ECH的同时测定。
Objective To establish a gas chromatographic method for the simultaneous determination of ethylene oxide (EO), propylene oxide (PO) and epichlorohydrin (ECH) in the workplace air. Methods The samples were collected by activated charcoal tube and desorbed by 5% (V / V) methanol-dichloromethane solution. The samples were separated by capillary column and detected by flame ionization detector. Results The mass concentration of EO, PO and ECH was 0.24 ~ 960.00, 0.60 ~ 2 384.00 and 0.12 ~ 472.40 mg / L, respectively. The correlation coefficient was 0.999 95 ~ 0.999 96. The minimum detectable concentrations were 0.06, 0.04 and 0.02 mg / m3, and the lowest quantification concentrations were 0.16,0.13 and 0.07 mg / m3, respectively. The average desorption efficiencies were 79.21% ~ 89.74%, 86.06% ~ 93.38% and 90.77% ~ 95.53%, respectively. The precision of the method was 2.52% ~ 3.68%, 1.64% ~ 3.09%, 2.15% ~ 3.53%, respectively. The precision among batches was 2.69% ~ 4.21%, 1.87% ~ 3.39%, 3.69% ~ 4.54%, respectively. EO, PO, and ECH samples were stored for at least 5, 7, and 7 d in a -20 ° C freezer, respectively. Conclusion The method has high sensitivity, good precision and simple operation. It is suitable for the simultaneous determination of EO, PO and ECH in the air of the workplace.