用于PM2.5样品测定的全反射X荧光仪的研制  

Developed of total reflection X-ray fluorescence spectrometer used for PM2.5 sample determination

作　　者：康海英[1] 郑维明[1] 崔大庆[1] 徐平 KANG Haiying;ZHENG Weiming;CUI Daqing;XU Ping(China Institute of Atomic Energy,Beijing 102413,China)

机构地区：[1]中国原子能科学研究院,北京102413

出　　处：《化学分析计量》2018年第2期112-116,共5页Chemical Analysis And Meterage

摘　　要：研制适用于PM2.5样品分析的Mo靶和W靶全反射X荧光仪(TXRF)。该仪器主要部分为光路和软件系统,经过光路系统的设计、加工、调试,使入射光达到全反射;软件开发实现了控制和数据获取处理功能。Mo靶TXRF测量各元素检出限(ng)分别为K 9.4,Ca 4.1,Sc 8.5,Ti 3.0,V 3.5,Cr 3.2,Mn 1.5,Fe 0.99,Ni 0.24,Cu 0.63,Zn 0.5,Pb1.6,Ba 11.9;W靶TXRF测量各元素检出限(ng)分别为Na 1 935,Mg 1 087,Al 1 310,K 19.4,Ca 8.8,Sc 7.0,Ti 13.5,V 7.8,Cr 2.3,Mn 4.0,Fe 4.5,Ni 4.5,Ba 6.2。重复测量100 ng的Ba和200 ng的Ti各6次,测定结果的相对标准偏差分别为5.3%,1.4%;51.2μg/cm2 Zn和9.0μg/cm2 Ca测量结果与标准值的相对偏差分别为0.2%,5.8%。用Mo靶、W靶TXRF分别连续测量标准薄膜Cu样和Fe样4 h,测定结果的相对极差分别为5.1%,6.0%。该仪器检测限低,测量重复性、准确度、长期稳定性均满足ng量级微量元素的测量需求,可用于大气微尘样品的直接测量。Total reflection X-ray fluorescence spectrometer(TXRF)instruments with Mo target and W target used for PM2.5 sample analysis were developed.The instruments include two important parts,the light path and software.Incident X-ray was totally reflected by designed and adjusted the light path.The instrument control and data collection and treatment were realized by using the newly developed software.The detection limits(ng)for the following elements by the TXRF instrument with W target are K 9.4,Ca 4.1,Sc 8.5,Ti 3.0,V 3.5,Cr 3.2,Mn 1.5,Fe 0.99,Ni 0.24,Cu 0.63,Zn 0.5,Pb 1.6,Ba 11.9.The detection limits(ng)for the following elements by the TXRF instrument with Mo target are Na 1 935,Mg 1 087,Al 1 310,K 19.4,Ca 8.8,Sc 7.0,Ti 13.5,V 7.8,Cr 2.3,Mn 4.0,Fe 4.5,Ni 4.5,Ba 6.2.For 6 times repeated measurements on 100 ng Ba and 200 ng Ti,the the relative standard deviations are 5.3%and 1.4%,respectively.For the measurements on 51.2 ng/cm2 Zn and 9.0 ng/cm2 Ca,the analytical errors are 0.2%and 5.8%,respectively.Continue measurements on Cu and Fe of air-filters by TXRF instruments with Mo target and W target,the relative differences are 5.1%and 6%,respectively.All of the parameters tested above proved that the newly developed TXRF instruments have low detection limits,can meet requirements of trace elements analysis for PM 2.5 particles collected on the air filter.

关 键 词：PM2.5样品 全反射X荧光仪 光路 软件 检出限 

分 类 号：O657.3[理学—分析化学]