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目的探讨适合工作场所空气中异佛尔酮的溶剂解吸气相色谱测定法中的解吸液,提高解吸效率。方法用活性炭管采样,硝基对苯二酸改性的聚乙二醇石英弹性毛细管柱(30.00 m×0.32 mm×0.25μm)分离,火焰离子化检测器检测,标准曲线法定量。采用不同的解吸液对异佛尔酮进行解吸,测定解吸效率。结果采用甲基异丁基甲酮(MIBK)解吸,平均解吸效率为83.8%,相对标准偏差(RSD)为3.2%;二硫化碳(CS2)解吸效率低于71%;MIBK解吸效率较CS2提高10%以上。以MIBK为溶剂的高、中、低水平异佛尔酮标准溶液重复测定RSD均小于1.0%;异佛尔酮在0.18～369.20 mg/L呈线性关系,回归方程y=0.920 00 x-0.802 22,相关系数=0.999 93;方法检出限为0.18 mg/L,以3L采样量计算对应于空气中的质量浓度为0.06 mg/m3,溶液和空气中的定量下限分别为0.61 mg/L和0.20 mg/m3。结论采用MIBK为解吸液,方法灵敏度、准确度高,解吸效率满足标准要求,可以应用于工作场所空气中异佛尔酮的测定。
Objective To explore the desorption solution suitable for solvent desorption gas chromatography of isophorone in the air of the workplace to improve the desorption efficiency. Methods Samples were taken from activated charcoal tube, separated on a nitrocellulose terephthalate - modified polyethylene glycol quartz capillary column (30.00 m × 0.32 mm × 0.25 μm), detected by flame ionization detector and quantified by standard curve method. Isophorone was desorbed using different desorption solutions and desorption efficiencies were determined. Results The desorption efficiency of MIBK was 83.8% with RSD of 3.2%. The desorption efficiency of CS2 was less than 71%. The desorption efficiency of MIBK was over 10% higher than that of CS2. The RSDs of isophorone standard solutions with high, medium and low levels of MIBK were less than 1.0%. The isophorone showed a linear relationship with 0.18 ~ 369.20 mg / L. The regression equation was y = 0.920 00 x-0.8022 , The correlation coefficient = 0.999 93; the detection limit of the method was 0.18 mg / L, which corresponded to a mass concentration of 0.06 mg / m3 in air with a sampling volume of 3L; the lower limits of quantitation in solution and air were 0.61 mg / L and 0.20 mg / m3. Conclusion MIBK was used as desorption solution. The sensitivity, accuracy and desorption efficiency meet the standard requirements and can be applied to the determination of isophorone in the air of workplace.