单波长激发-能量色散X射线荧光光谱法测定含铁物料中多种微量及痕量有害元素  

Determination of Various Trace and Harmful Elements in Iron Containing Materials by Single Wavelength Excitation Energy Dispersive X-ray Fluorescence Spectrometer

作　　者：杨金坤 苏明跃 李权斌 臧世阳 韩伟丹 YANG Jinkun;SU Mingyue;LI Quanbin;ZANG Shiyang;HAN Weidan(Tianjin Customs Chemical and Mineral Metal Material Testing Center,Tianjin 300457,China;Tianjin Customs Industrial Product Safety Technology Center,Tianjin 300457,China;Beijing Ancoren Science&Technology Co.,Ltd.,Beijing 065500,China)

机构地区：[1]天津海关化矿金属材料检测中心,天津300457 [2]天津海关工业产品安全技术中心,天津300457 [3]北京安科慧生科技有限公司,北京065500

出　　处：《中国无机分析化学》2024年第9期1227-1233,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：海关总署科研项目(2021HK218);国家重点研发计划项目(2017YFF0108905)。

摘　　要：采用全聚焦型双曲面弯晶结构所实现的单波长激发能量色散X射线荧光光谱法,能有效解决X射线管出射谱中韧致辐射所产生的背景信号,大幅提升元素信噪比,获得较佳的元素特征X射线荧光信号峰背比,降低检出限,可定量分析含铁物料中多种微量及痕量有害元素。称取适量铁矿样品制备成粉末压片,通过对单波长激发性能进行优化,以基本参数法对基体效应进行校正,采用无标样全谱拟合算法对试样进行分析,砷、汞、铅、铬、镉元素的线性相关系数均不小于0.999,其检出限在0.0002%~0.003%,各元素精密度RSD在3.2%~9.0%。用不同方法进行正确度验证,除接近方法检测下限的As及Pb检测结果与对比数据偏差较大之外,其他元素与比对方法的测定结果均吻合。经实验表明,采用双曲面弯晶技术的单波长激发能量色散X射线荧光光谱法定量分析含铁物料中低含量有害元素,正确度高、检出限低,明显优于传统能量色散X射线荧光光谱法。The single wavelength excitation energy dispersive X-ray fluorescence spectroscopy achieved by using a fully focused hyperbolic curved crystal structure can effectively solve the background signal generated by bremsstrahlung in the X-ray tube emission spectrum,significantly improve the element signal-to-noise ratio,obtain better peak to back ratio of element characteristic X-ray fluorescence signals and reduce the detection limit.Various trace and harmful elements in iron containing materials can be quantitatively analyzed by this measurement.an appropriate amount of iron ore samples was weighed and prepared into powder tablets.The single wavelength excitation performance was optimized,and the matrix effect using the basic parameter method was corrected,and the sample using the standard free full spectrum fitting algorithm was analyzed.The linear correlation coefficients of arsenic,mercury,lead,chromium,and cadmium elements were not less than 0.999,with a detection limits of 0.0002%to 0.003%and a precision RSD of 3.2%to 9.0%.Using different methods for accuracy verification,except for the As and Pb element detection results close to the lower limit of the method with significant deviation from the comparison data,the determination results of other elements were consistent with the comparison method.Experimental results have shown that the single wavelength excitation energy dispersive X-ray fluorescence spectroscopy using hyperbolic curved crystal technology for quantitative analysis of low content harmful elements in iron containing materials has high accuracy and low detection limit,which is significantly better than traditional energy dispersive X-ray fluorescence spectroscopy.

关 键 词：单波长激发 能量色散 X射线荧光光谱法 含铁物料 有害元素 

分 类 号：O657.34[理学—分析化学]