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目的建立溶剂解吸—气相色谱测定工作场所空气中二氯甲烷的检测方法。方法采用溶剂解吸型活性炭管进行采样,二硫化碳解吸,毛细管柱进行分离,氢焰离子化检测器检测,保留时间定性,峰高或峰面积定量。依据“工作场所空气中毒物检则方法的研究规范”的要求,对方法进行实验室研究验证。结果在样品测定条件下,标准曲线线性范围在25～4000μg/ml之间,相关系数在0.999以上;检出限为1.2μg/ml;相对标准偏差(RSD)在1.87%～4.36%之间;加标回收率在98.5%～99.2%之间;采样效率在91.0%～97.6%之间;穿透容量大于2.0 mg;平均解吸效率为90.3%;样品在室温下至少可保留7 d。结论该方法各项实验室验证指标均符合“《工作场所空气中毒物检测方法的研究规范(原WS/T73-1996)》”的要求,经过在检测与评价工作中应用,证实该方法可以用于工作场所空气中有毒物质二氯甲烷的测定。
Objective To establish a method for the determination of methylene chloride in the air by solvent desorption-gas chromatography. Methods Solvent desorption activated carbon tube was used for sampling, carbon disulfide desorption, capillary column separation, hydrogen flame ionization detector detection, retention time qualitative, peak height or peak area quantification. According to “workplace air poisoning inspection method research code ” requirements, the method of laboratory research and verification. Results The linear range of the standard curve was between 25 and 4000 μg / ml with the correlation coefficient above 0.999. The detection limit was 1.2 μg / ml. The relative standard deviations (RSDs) ranged from 1.87% to 4.36% The spiked recoveries ranged from 98.5% to 99.2%. The sampling efficiencies ranged from 91.0% to 97.6%. The breakthrough capacities were above 2.0 mg. The average desorption efficiency was 90.3%. The samples were preserved for at least 7 days at room temperature. Conclusion All the laboratory verification indexes of this method are in accordance with the requirements of the research standard of the workplace air poisoning detection method (formerly WS / T73-1996) “”. After the application in testing and evaluation, it is proved that this method Can be used for determination of dichloromethane in workplace air toxic substances.