大气PM_(2.5)采样滤膜中16种元素的动态反应池-电感耦合等离子体质谱测定法

Direct determination of 16 metals on air particulate filter membrane by ICP-DRC-MS

目的采用动态反应池(DRC)技术消除质谱干扰,对电感耦合等离子体质谱(ICP-MS)法测定大气PM_(2.5)采样石英滤膜中16种化学元素的方法进行改进。方法应用单因素试验设计,对反应气(氨气)流量和Rpq等DRC模式相关条件进行优化,随后对经混合酸体系微波消解法处理后的石英滤膜样品进行检测,并配合在线内标法对质谱干扰进行校正。结果除砷和硒元素外,本方法对其余14种元素检出限均优于标准模式(STD)方法,符合《空气污染物对人群健康影响监测工作手册(2016版)》规定的方法学要求。测定过滤介质大气颗粒物2783标准参考物显示,测定结果均在理论值范围内,精密度为3.4%~9.4%。结论改进方法能有效消除谱线干扰、基体干扰和物理干扰等,适合同时测定大气颗粒物中16种化学元素,可满足日常样品的检测需求。

Objective To establish a method for the determination of 16 metals on air particulate filter membrane by inductively coupled plasma-dynamic reaction cell-mass spectrometry（ICP-DRC-MS）. Methods A single factor experimental design was used to optimize the reaction gas flow and Rpq, then the samples were treated with mixed acid system of microwave digestion method and determined. The interference of mass spectra was corrected with internal standardization and DRC system to eliminate.Results The method could eliminate spectral interferences, matrix interferences and physical interferences. In addition to As and Se, the limits of detection of the other 14 elements were better than those of the STD model. The method was applicable to the methodological requirements of the Handbook of Air Pollution Affecting Human Health Monitoring（2016 edition）. The determination of standard reference material（STANDARD REFERENCE MATERIAL~ 2783） showed that the measured results were within the theoretical range and the relative standard deviation（RSD） were between 3.4%-9.4%. Conclusion The improved method is applicable to the simultaneous determination of 16 metals on air particulate filter membrane.