工作场所空气中乙酰丙酮测定的溶剂解吸-气相色谱法

Determination of acetylacetone in workplace air by solvent desorption-gas chromatography

目的建立工作场所空气中乙酰丙酮的气相色谱测定法。方法于2020年8月,以硅胶管采集工作场所空气中的乙酰丙酮,用甲醇解吸,经毛细管色谱柱分离,火焰离子化检测器检测,并对方法的检出限和精密度等指标进行分析。结果乙酰丙酮在1.95~1950.60μg/ml内线性关系良好,回归方程为y=0.815x-3.667,相关系数为0.99993,检出限为0.18μg/ml,最低检出浓度为0.12 mg/m^(3)(空气体积以1.50 L计算);批内精密度为1.08%~4.11%,批间精密度为1.98%~2.80%,解吸效率为99.68%~100.45%;样品在室温下至少可以保存15 d。结论乙酰丙酮的溶剂解吸-气相色谱测定法精密度好,灵敏度高,操作简单,适用于工作场所空气中乙酰丙酮的测定。

Objective To establish a method for the determination of acetylacetone in the air of workplace by gas chromatography.Methods In August 2020,acetylacetone in the air of workplace was collected by silica gel tube,eluted with methanol,separated and detected by gas chromatography with flame ionization detector.The detection limit and precision of the method were also analyzed.Results The linear range of acetylacetone was 1.95-1950.60μg/ml with the regression equation of y=0.815x-3.667,and the correlation coefficient was 0.99993.The limit of detection of the method was 0.18μg/ml and the minimum detection concentration was 0.12 mg/m^(3)(collected sample volume was 1.50 L).The within-run precisions were 1.08%-4.11%and the between-run precisions were 1.98%-2.80%.The desorption rates were 99.68%-100.45%.The sealed samples could be kept at least 15 days at room temperature without significant loss.Conclusion The solvent desorption-gas chromatography method for the determination of acetylacetone has good precision,high sensitivity and simple operation,and is suitable for the determination of acetylacetone in the air of the workplace.