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[目的]使用混合溶剂提高空气中异佛尔酮的溶剂解吸气相色谱测定法中的解吸效率。[方法]活性炭管采样后,10%(体积分数)异丙醇-二硫化碳混合溶剂解吸,聚乙二醇石英弹性毛细管柱INNOWAX(30.0 m×0.53 mm×1.0μm)分离,火焰离子化检测器检测,保留时间定性、标准曲线外标法定量。[结果]10%异丙醇-二硫化碳混合溶剂解吸活性炭中异佛尔酮,平均解吸效率为92.6%。浓度分别为10、60、150 mg/L的异佛尔酮加标样品测定结果显示批内、批间相对标准偏差分别<5%、10%。异佛尔酮在0.28~400 mg/L呈线性关系,回归方程y^=1.947x-0.904,相关系数r=1.000 0;方法检出限为0.084 mg/L。以2.5 L采样量计算,异佛尔酮的最低检出浓度为0.034 mg/m3,最低定量浓度为0.11 mg/m3。[结论]采用10%异丙醇-二硫化碳混合溶剂为解吸剂,其解吸效率高于仅使用二硫化碳(<70%)。该方法应用于工作场所空气中异佛尔酮的测定,方法精密度、准确度良好,解吸效率满足相关国家标准要求。
[Purpose] To improve the desorption efficiency of isophorone in air by solvent desorption gas chromatography using a mixed solvent. [Method] After the activated carbon tube was sampled, 10% (volume fraction) isopropanol - carbon disulfide mixed solvent was desorbed, and polyethylene glycol - silica capillary column INNOWAX (30.0 m × 0.53 mm × 1.0 μm) was used for separation. Flame ionization detector , Retention time qualitative, standard curve external standard method. [Result] Isophorone was desorbed in 10% isopropanol - carbon disulfide mixed solvent, and the average desorption efficiency was 92.6%. The determination of isophorone spiked at concentrations of 10, 60 and 150 mg / L, respectively, showed that the relative standard deviations (RSDs) were <5% and 10% respectively. Isophorone was linear in the range of 0.28-400 mg / L, the regression equation was y = 1.947x-0.904, the correlation coefficient was 1.000 0, and the detection limit was 0.084 mg / L. The minimum detectable concentration of isophorone was 0.034 mg / m 3 and the lowest quantified concentration was 0.11 mg / m 3 at 2.5 L sample volume. [Conclusion] The desorption efficiency of 10% isopropanol-carbon disulfide solvent was higher than that of carbon disulfide alone (<70%). The method is applied to the determination of isophorone in the air of the workplace, the method has good precision and accuracy, and the desorption efficiency meets the requirements of relevant national standards.