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目的研究建立工作场所空气中异亚丙基丙酮的溶剂解吸气相色谱测定方法。方法用活性炭采样管采样,二硫化碳(CS2)解吸,DB-WAX毛细管柱分离,氢火焰离子化检测器(FID)检测。结果在选定实验条件下,异亚丙基丙酮在0.015~3.600 g/L之间线性关系良好,相关系数(r)=0.999 7;日内精密度为0.40%~2.06%,日间精密度为1.18%~2.24%;加标回收率为96.36%~110.70%(n=18);方法检出限为0.001 87 g/L;最低检出浓度为0.623 mg/m3(以采样体积3.0 L空气计);采样效率为98.21%~99.50%;解吸效率为87.96%~93.86%;穿透容量为4 h 11.29 mg(100 mg活性炭);样品稳定性为4℃下第10天样品下降率为3.1%。结论该方法线性范围宽,灵敏度高,精密度、准确度好,样品采集简便,采样结果稳定,达到工作场所空气中有毒物质检测方法的研制规范要求,适用于工作场所空气中异亚丙基丙酮浓度的监测。
Objective To establish a gas chromatography method for the determination of mesityl oxide in workplace air by solvent desorption. Methods The samples were taken from activated carbon sampling tube, carbon disulfide (CS2) desorption, DB-WAX capillary column separation and hydrogen flame ionization detector (FID). Results Under the selected experimental conditions, the linear relationship of isopropylidene acetone between 0.015 and 3.600 g / L was good with the correlation coefficient (r) = 0.999 7; the intra-day precision was 0.40% ~ 2.06% 1.18% ~ 2.24%. The spiked recoveries ranged from 96.36% to 110.70% (n = 18). The detection limit was 0.001 87 g / L and the lowest detection limit was 0.623 mg / ); The sampling efficiency was 98.21% -99.50%; the desorption efficiency was 87.96% -93.86%; the breakthrough capacity was 4 h 11.29 mg (100 mg activated carbon); the sample stability was 3.1% at 4 ℃, . Conclusion The method has the advantages of wide linear range, high sensitivity, good precision and accuracy, simple sample collection and stable sampling results. It meets the requirements of the research and development standards for the detection of toxicants in the air in the workplace. It is suitable for the application of isopropylidene acetone Concentration monitoring.