气相色谱法测定工作场所空气中乙酸仲己酯方法的研究

Methods for determination of sec-hexyl acetate in air of workplace by GC

目的:建立工作场所空气中乙酸仲己酯(1,3-二甲基丁基醋酸酯)的气相色谱测定方法。方法:根据乙酸仲己酯的理化性质和在空气中存在状态,参考NIOSH分析方法,选用活性炭管采集样品,二硫化碳解吸,经FFAP柱分离,用氢火焰离子化检测器测定。结果:本研究方法测定工作场所空气中乙酸仲己酯线性范围9.35～23400μg/ml,回归方程Y=0.0264X-156.5,相关系数均值r=0.9996。最低检出限为1.4μg/ml,检测下限2.33μg/ml,检出浓度为1.6 mg/m3(以采集1.5 L空气样品计)。相对标准偏差(RSD)分别为3.3%、2.7%和3.9%,解吸效率均值分别为99.2%、99.9%%和99.1%;穿透容量在100 mg活性炭上大于32 mg;乙酸仲己酯在室温下至少可保存15 d;采样效率为100%。结论:建立了工作场所空气中乙酸仲己酯(1,3-二甲基丁基醋酸酯)的气相色谱测定方法,具有灵敏度高、操作简便、重现性好、准确可靠,适合检测工作场所空气中乙酸仲己酯(1,3-二甲基丁基醋酸酯)的浓度。

Objective：A method for the quantitative determination of sec-hexyl acetate（1,3-dimethylbutyl acetate） in the air of workplace was developed with reference to NIOSH 1450.Methods：In order to do so,various procedures for the samping and measurement were tested.A methodology was developed which included samping with acticarbon tube,desorbing with carbon disulfide,chromatographic separation by FFAP capillary column and determination by GC-FID.Results：The analytical features of the method are as follows： linear relationship range,9.35~23400 μg/ml;regression equation,Y=0.0264X-156.5;the mean of correlation coefficient,r=0.9996;detection limit,1.6 mg/m3（1.5 L air volume sampled）;precision（RSD）,2.7%~3.9%;desorption efficiency（DE）,99%;breakthrough volume,32 mg（100 mg coconut shell charcoal）;Storage Stability,〉15days（room temperature）;sampling efficiency,100%.Conclusion：It is suitable for analysis of the concentration of sec-hexyl acetate（1,3-dimethylbutyl acetate） in the air of workplace due to its satisfactory accuracy and precision according with the requirement of workplace analysis.It is a simple,rapid and practical analytical technique.