摘要
目的建立工作场所空气中苯胺的毛细管气相色谱法。方法采用硅胶管采集工作场所中空气样品,无水乙醇解吸,应用HP-5毛细管色谱柱,采用程序升温方式进行分离,火焰离子检测器检测,保留时间定性,外标法定量。结果本法采用HP-5毛细管色谱柱分离苯胺效果良好,在2μg/ml^500μg/ml浓度内,苯胺的浓度与峰面积呈良好的线性关系,线性方程为y=13 540.2x-455.9,相关系数(r)为0.999 9,检出限为0.06 mg/L,定量限为0.21 mg/L;当采集3 L工作场所空气时,最低检出浓度为0.02 mg/m3。室温下,解吸时间为10 min时,平均解吸效率为88.4%~97.3%,相对标准偏差(RSD)为1.0%~2.6%。样品于4℃冰箱内至少可稳定保存14 d。结论该方法分离效果好,线性范围宽,精密度高,分析时间短,适用于工作场所空气中苯胺的检测。
Objective To establish a method for the determination of aniline in workplace air by solvent desorption capillary gas chromatography. Methods The air samples were collected with silica gel tubes,then desorbed with absolute ethanol,separated with HP-5 capillary column by programmed heating,and detected by flame ionization detector（ FID）. Qualitative analysis was based on retention time and quantitative analysis was based on peak area standard curve. Results The method showed a good separation effect by HP-5 capillary column. The concentrations of aniline presented a good linear relationship with peak area within the range of 2 μg/ml-500 μg/ml,the linear equation was y = 13 540. 2 x-455. 9,and the correlation coefficient（ r） was0. 999 9. The limit of detection was 0. 06 mg/L,and the quantitation limit was 0. 21 mg/L. The lowest detection limit of method was 0. 02 mg/m3,when the sampling volume was 3 L. When the desorption time was 10 min,the efficiency of desorption was within 88. 4%-97. 3%,with the relative standard deviation（ RSD） of 1. 0%-2. 6%. The samples could be stable for over 14 days in refrigerator at 4 ℃. Conclusion The method was efficient in separation,wide linear,accurate and time-saving and it is suitable for the determination of aniline in workplace air.
出处
《中国卫生检验杂志》
CAS
2017年第23期3372-3373,3376,共3页
Chinese Journal of Health Laboratory Technology
