模拟大气颗粒物混合元素滤膜标准样品的研制与质量考察  

Development and quality inspection of standard samples of simulated atmospheric particulate mixed elements filter membrane

作　　者：杜祯宇 张百慧 黄智鹏 张轩雄 黄冲 李玉武 DU Zhen-yu;ZHANG Bai-hui;HUANG Zhi-peng;ZHANG Xuan-xiong;HUANG Chong;LI Yu-wu(Environmental Development Centre of the Ministry of Ecology and Environment,Beijing 100029,China;National Research Center for Environmental Analysis and Measurements,Beijing 100029,China;State Environmental Protection Key Laboratory for Dioxin Pollution Control,Beijing 100029,China;Guohuan Oasis(Gu′an)Environmental Technology Co.,Ltd.,Langfang 065500,China;School of Chemical Science and Technology,Tongji University,Shanghai 200092,China;School of Optical and Electronic Information Engineering,University of Shanghai for Science and Technology,Shanghai 200093,China;Skyray Instrument,Kunshan 215300,China)

机构地区：[1]生态环境部环境发展中心,北京100029 [2]国家环境分析测试中心,北京100029 [3]国家环境保护二噁英污染控制重点实验室,北京100029 [4]国环绿洲(固安)环境科技有限公司,河北廊坊065500 [5]同济大学化学科学与化工学院,上海200092 [6]上海理工大学光学与电子信息工程学院,上海200093 [7]天瑞仪器股份有限公司,江苏昆山215300

出　　处：《冶金分析》2020年第11期1-7,共7页Metallurgical Analysis

基　　金：大气重污染成因与治理攻关项目(No.DOGG0306);国家重点研发计划项目(2016YFC0208104)。

摘　　要：用能量色散X射线荧光光谱法(ED-XRF)测定大气颗粒物滤膜样品中Na、Mg、Al、Si、P、S、Cl、K、Ca、Ti、V、Cr、Mn、Fe、Co、Ni、Cu、Zn、As、Pb、Sr、Ba等无机元素的HJ 829—2017标准已颁布实施多年。颗粒物滤膜标准样品对于校准曲线的建立、评估具有重要意义。目前市场仅有美国NIST SRM 2783一种模拟大气颗粒物滤膜标准样品,价格昂贵,基层实验室在日常检测工作中很难用于质控工作。没有价格合适、质量符合要求相关产品投放市场,基层实验室大气颗粒物元素XRF分析质控工作就无法落实。借鉴国外模拟大气颗粒物滤膜标样制备方法,以湖南污染土壤标样为加工原材料,经进一步粉碎后,利用表面活性剂将细颗粒物制成悬浊液,定量、均匀分布在多孔滤膜上。6家ED-XRF实验室,1家质子激发X荧光光谱分析(PIXE)和1家中子活化分析(NAA)实验室,对同批次制备的120张滤膜样品随机抽取14张进行了测试,对滤膜上20多种元素测定结果的准确度和精密度进行了评估。初步分析结果表明:Al、Fe、Zn、As、Ba、Ti、Pb等元素含量与依据土壤标样元素认定值比值推算的结果基本相符;Al、Si、Fe、Ti、Mn、Zn、K、As、Pb等元素含量相对标准偏差(RSD)范围为6.8%~21%,基本满足滤膜质控样品要求,可以提供给基层实验室试用。提出了后续研究工作思路及计划。The standard of HJ 829-2017,which is concerning the determination of inorganic elements such as Na,Mg,Al,Si,P,S,Cl,K,Ca,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,As,Pb,Sr and Ba in atmospheric particulate filter membrane sample by energy dispersive X-ray fluorescence spectrometry(EDXRF),has been issued and implemented for several years.The standard sample of particulate filter membrane is of great significance for the establishment and evaluation of calibration curves.At present,there is only one standard sample for simulating particulate filter membrane(NIST SRM 2783,USA)in the market.But the price is expensive,and it is difficult to be used in quality control for the primary-level laboratories in routine analysis.If there is no relevant product with appropriate price and quality that meets the requirements,the quality control of XRF analysis for the testing of atmospheric particulate elements will be hardly implemented in primary-level laboratories.Refer to the preparation method of foreign simulated atmospheric particulate filter membrane,the standard sample of polluted soil sampled from Hunan was used as raw materials.After further pulverization,the fine particles were made into a suspension by using surfactant.Then the suspension was quantitatively and uniformly distributed on the porous filter membrane.Total 120 pieces of filter membrane samples were prepared in one batch and 14 of them were randomly selected for testing by 6 ED-XRF laboratories,one proton induced X-ray emission(PIXE)laboratory and one neutron activation analysis(NAA)laboratory.The determination accuracy and precision of measuring results of more than 20 elements on filter membrane were evaluated.The preliminary analysis results showed that the contents of Al,Fe,Zn,As,Ba,Ti and Pb were basically consistent with the results calculated based on the ratio of certified values of elements in soil standard sample.The relative standard deviations(RSD)of Al,Si,Fe,Ti,Mn,Zn,K,As and Pb were between 6.8%and 21%,which could basically meet the requirements of filter me

关 键 词：大气颗粒物 模拟样品 无机元素 滤膜标准样品 能量色散X射线荧光光谱 质子激发X荧光光谱 中子活化分析 

分 类 号：O657.34[理学—分析化学]