工作场所空气中二氯甲烷的溶剂解吸—气相色谱测定法

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。

Solvent Desorption-Gas Chromatography in Determining Dichlormethane in Workplace Air

[Objective]To establish the determination of dichlormethane in workplace air by solvent desorption-gas chromatography.[Methods]The samples were collected by solvent desorption activated carbon tube,desorbed by carbon disulfide,separated by capillary column,determined by hydrogen flame ionization detector to retain the qualitative time and the quantitative climax,according to the requirements of ＂research standard about the methods for determination of toxic substance in workplace air＂,the method was verified by lab research.[Results]Under the condition of sample determination,the linear range of the standard curve was between 25～4000 μg/ml,correlation coefficients was above 0.999,the detection limit was 102 μg/ml,relative standard deviation（RSD）was between 1.87%～4.36%,the recovery of standard addition was between 98.5%～99.2%,sampling efficiency was between 91.0%～97.6%,breakthrough volume was above 2.0 mg,the average desorption efficiency was 90.3%,and samples could be retained for at least 7 days at room temperature.[Conclusion]Laboratory validated indicators of this method accord with the requirements of ＂research standard about the methods for determination of toxic substance in workplace air＂（formal WS/T 73-1996）,and by the application in the testing and evaluation,this method is proved to be used in determining dichloromethane in workplace air.