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目的建立工作场所空气中毒死蜱的溶剂解吸气相色谱测定方法。方法按照《工作场所空气中有毒物质检测方法研究规范》的相关要求进行实验。采用OVS-2管采集工作场所空气中毒死蜱等有机磷农药,用溶剂(取90 ml甲苯和10 ml丙酮混合)解吸后,经DB-1701气相色谱柱分离,火焰光度检测器进行检测。结果本方法在0～10.0 mg/L呈线性关系(r=0.999 93),样品在吸附管中可保存13 d,不同质量浓度样品测定的相对标准偏差为0.49%～1.50%,方法的最低检出限为0.005 mg/L,定量下限为0.017 mg/L,方法的最低检出质量浓度为0.002 mg/m3,平均解吸效率为99.3%～100.1%,采样效率为99.4%～100.0%,加标回收率为98.2%～99.2%,空气中与毒死蜱共存的敌敌畏、甲胺磷、乐果、甲拌磷、毒死蜱、甲基对硫磷、马拉硫磷、对硫磷、甲基毒死蜱等有机磷在本方法条件下不干扰测定。结论此方法各项指标均达到《工作场所空气中有毒物质检测方法研究规范》的要求,适用于工作场所空气中毒死蜱和其他有机磷农药的现场监测。
Objective To establish a method for the determination of chlorpyrifos in the workplace by gas chromatography with solvent desorption. Methods The experiment was conducted in accordance with the relevant requirements of the “Study Norms for the Detection of Toxic Substances in the Air at Work”. The OVS-2 tube was used to collect organophosphorus pesticides in the air, such as chlorpyrifos in the air, desorbed with solvent (mixed with 90 ml of toluene and 10 ml of acetone), separated by DB-1701 gas chromatograph and detected by flame photometric detector. Results The method was linear in the range of 0-10.0 mg / L (r = 0.999 93). The sample was stored in the adsorption tube for 13 days. The relative standard deviations (RSDs) were 0.49% -1.50% for different concentration samples. The method was the lowest The limit of detection was 0.005 mg / L and the limit of quantitation was 0.017 mg / L. The minimum detectable concentration was 0.002 mg / m3. The average desorption efficiency was 99.3% ~ 100.1% and the sampling efficiency was 99.4% ~ 100.0% The recoveries ranged from 98.2% to 99.2%. The organic solvents such as dichlorvos, methamidophos, dimethoate, phorate, chlorpyrifos, methyl parathion, malathion, parathion and chlorpyrifos- Phosphorus does not interfere with the assay under the conditions of this method. Conclusion The indexes of this method all meet the requirements of the “Research Criteria for Detection of Toxic Substances in the Air at Workplace” and are suitable for on-site monitoring of chlorpyrifos and other organophosphorus pesticides in the air in the workplace.