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目的建立工作场所空气中氯甲甲醚(CMME)和双氯甲醚(BCME)的气相色谱测定方法。方法空气中的CMME和BCME经吸收液采集后,经衍生化处理,衍生产物在碱性条件下用正己烷萃取,毛细管色谱柱分离,电子捕获检测器检测,标准曲线法定量。结果本方法测定CMME和BCME的质量分别在2.00~80.00和1.32~52.80 ng时线性关系良好,线性相关系数均为0.999 93;最低检出浓度均为0.030μg/m3,最低定量浓度均为0.100μg/m3(以采集7.50 L空气计);加标回收率分别为99.35%~101.00%和97.99%~101.70%;批内相对标准偏差(RSD)分别为2.73%~4.46%和2.61%~3.82%,批间RSD分别为3.10%~5.50%和3.89%~5.38%;采样效率分别为92.43%~96.25%和91.43%~94.03%;CMME和BCME样品在室温下至少可储存15 d。结论本方法适用于工作场所空气中CMME和BCME的检测。
Objective To establish a gas chromatographic method for the determination of chlormethylethylene (CMME) and bichloromethylether (BCME) in workplace air. Methods CMME and BCME in the air were collected by absorption solution and derivatized. The derivatized products were extracted with n-hexane under basic conditions, separated by capillary column, detected by electron capture detector and quantified by standard curve method. Results The linearity of CMME and BCME from 2.00 to 80.00 and from 1.32 to 52.80 ng were determined by this method. The linear correlation coefficients were both 0.999 93. The minimum detectable concentrations were both 0.030 μg / m 3 and the lowest concentrations were 0.100 μg / m3 for 7.50 L air, the recoveries of standard addition ranged from 99.35% to 101.00% and from 97.99% to 101.70%, respectively. The relative standard deviations (RSDs) were 2.73% -4.46% and 2.61% -3.82% The inter-assay RSD was 3.10% -5.50% and 3.89% -5.38% respectively. The sampling efficiencies were 92.43% -96.25% and 91.43% -94.03%, respectively. The CMME and BCME samples were stored for at least 15 days at room temperature. Conclusion This method is suitable for the detection of CMME and BCME in the workplace air.