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目的建立工作场所空气中环氧丙烷(PO)、环氧氯丙烷(ECH)的溶剂解吸气相色谱同时测定法。方法采用活性炭管采样,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(FID)测定PO、ECH质量浓度。并同时进行解吸效率、精密度、采样效率、穿透容量、样品稳定性、干扰试验等对该方法进行评价。结果 PO、ECH质量浓度分别在2.07~414.00、0.354~70.800 mg/L线性关系良好,相关系数均为0.999 9,检出限分别为0.20、0.06 mg/L、定量下限分别为0.60、0.20 mg/L(分别以3、10倍标准差计算),最低检出质量浓度分别为0.07、0.02 mg/m3、最低定量质量浓度分别为0.20、0.07 mg/m3(以采集3.0 L空气计)。方法批间精密度相对标准偏差(RSD)分别为4.30%~6.00%、1.51%~6.57%,平均解吸效率分别为77.9%~82.1%、92.1%~94.4%。PO、ECH样品在-20℃冰箱中分别可保存5、7 d。结论该法操作简单,灵敏度高,精密度好,适用于工作场所空气中PO、ECH的同时测定。
Objective To establish a method for the simultaneous determination of propylene oxide (PO) and epichlorohydrin (ECH) in workplace air by solvent desorption gas chromatography. Methods Activated carbon tube was sampled and desorbed in 5% (v / v) methanol - methylene chloride solution. The mass concentration of PO and ECH was determined by capillary gas chromatography and hydrogen flame ionization detector (FID). At the same time, the method was evaluated for desorption efficiency, precision, sampling efficiency, penetration capacity, sample stability, interference test and the like. Results The linear range of PO and ECH was 2.07 ~ 414.00 and 0.354 ~ 70.800 mg / L respectively, the correlation coefficients were 0.999 9, the detection limits were 0.20 and 0.06 mg / L, the lower limits of quantitation were 0.60 and 0.20 mg / L (respectively, 3,10 times the standard deviation), the lowest detected mass concentrations were 0.07,0.02 mg / m3, the lowest quantitative mass concentrations were 0.20,0.07 mg / m3 (to collect 3.0 L air meter). The relative standard deviations (RSDs) of the methods were between 4.30% -6.00% and 1.51% -6.57%, respectively. The average desorption efficiencies were 77.9% -82.1% and 92.1% -94.4%, respectively. PO, ECH samples were stored in -20 ℃ refrigerator for 5,7 d. Conclusion The method is simple, sensitive and accurate, suitable for the simultaneous determination of PO and ECH in the air of the workplace.