偏振X射线荧光分析尾矿薄层样品的散射校正方法研究  

Study on Sample Preparation Method of Plant Powder Samples for Total Reflection X-Ray Fluorescence Analysis

作　　者：贾文宝[1] 李俊[1] 张新磊[1] 杨晓艳 邵金发 陈齐炎 单卿[1] 凌永生[1] 黑大千 JIA Wen-bao;LI Jun;ZHANG Xin-lei;YANG Xiao-yan;SHAO Jin-fa;CHEN Qi-yan;SHAN Qing;LING Yong-sheng;HEI Da-qian(Department of Nuclear Science and Technology,College of Materials Science and Technology,Nanjing University of Aeronautics and Astronautics,Nanjing 211106,China;Inner Mongolia Institute of Metrology and Testing,Huhhot 010030,China;Key Laboratory of Ray Beam Technology of Ministry of Education,College of Nuclear Science andTechnology,Beijing Normal University,Beijing 100875,China;School of Nuclear Science and Technology,Lanzhou University,Lanzhou 730000,China)

机构地区：[1]南京航空航天大学材料科学与技术学院,核科学与技术系,江苏南京211106 [2]内蒙古自治区计量测试研究院,内蒙古呼和浩特010030 [3]北京师范大学核科学与技术学院,射线束技术教育部重点实验室,北京100875 [4]兰州大学核科学与技术学院,甘肃兰州730000

出　　处：《光谱学与光谱分析》2023年第1期169-174,共6页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(11975121,U1930125,12105143)资助。

摘　　要：了解尾矿浆中的重金属元素含量能为矿物浮选提供决策依据,不仅可以提高矿物的利用率,还可减少环境污染。X射线荧光光谱法是一种常用的重金属元素分析技术,对于地质类样品的分析,康普顿散射内标法是一种常用的定量方法。但对于薄层沉积样品,其康普顿散射峰强度会受到支撑滤膜的散射影响。由于样品紧密附着在支撑滤膜上,难以直接获得来自样品本身的康普顿散射强度,不利于直接应用康普顿散射峰强度进行定量分析。以尾矿薄层样品为分析对象,研究了不同聚丙烯滤膜厚度对康普顿散射峰强度的影响,并对薄层样品的康普顿散射强度进行了校正。实验结果表明,在0.34~3.06 mm厚度范围内,康普顿散射峰强度随聚丙烯滤膜厚度的增加线性增加,通过建立探测器获得的总康普顿散射强度与滤膜厚度的线性关系,计算出样品的净康普顿散射峰强度。为验证该修正方法的可靠性,利用蒙特卡洛方法模拟研究了无滤膜的尾矿样品和带有不同厚度滤膜的尾矿样品,结果显示经滤膜厚度影响修正后的净康普顿散射峰强度与无滤膜样品康普顿散射峰强度基本一致,相对偏差为0.41%。同时通过实验和模拟计算了0.34 mm厚聚丙烯滤膜时修正后的净康普顿散射峰强度占总康普顿散射峰的比例,分别为91.31%和89.91%,二者基本一致。最后,利用了上述基于滤膜厚度康普顿散射影响的校正方法,建立了基于康普顿散射内标法的定量校准曲线,对两种尾矿浆中的Cu,Zn和Pb元素的定量分析结果显示,未经滤膜厚度修正的康普顿内标校正相比校正前,部分元素定量结果与ICP-OES结果相比,其相对偏差反而增加3.18%~9.00%。而经滤膜厚度修正的康普顿内标方法的定量结果与ICP-OES结果的相对误差在1.14%~11.15%之间,相比于校正之前,相对偏差减少了0.30%~8.97%。The knowledge of tailing slurry’s heavy metal elementalry grade is important in mineral flotation processing.It can improve mineral utilization andreduce environmental pollution.X-ray fluorescence spectroscopy is an effective technology for determining heavy metal elements.Compton scattering internal standard is commonly used in X-ray fluorescence spectroscopy quantitation for geological samples.However,for thin film samples,the Compton scattering peak will be affected by the filter.However,it wasn’t easy to measure the Compton scattering intensity of the sample directly because it was tightly attached to the filter.In this paper,the filter’s influence on the sample’s Compton scattering intensity was discussed for the tailing slurry’s thin film sample after filtration,and the Compton scattering intensity of the thin film sample was corrected.The experimental results show that the intensity of the Compton scattering peak increases linearly with the increase of the thickness of the polypropylene filterin the thickness range of 0.34~3.06 mm.Therefore,the linear relationship between the total Compton scattering intensity obtained by the detector and the filter thickness was established,and the scattering peak intensity was the true Compton scattering peak intensity of the sample when the filter thickness was 0.Afterwards,Monte Carlo simulated the Compton scattering of samples with no filter and samples with different filter thicknesses.The results showed that the corrected Compton scattering intensity was the same as that of the sample without filter,with a relative deviation of only 0.41%.The ratio of the corrected Compton scattering intensity to the uncorrected Compton scattering peak were 91.31%and 89.91%,compared through experiments and simulations when the thickness ofthe polypropylene filter is 0.34 mm,which has a good consistency.Finally,the standard curves of elements were established and corrected by the uncorrected and corrected Compton scattering internal standards after six standard materials we

关 键 词：偏振X射线荧光光谱分析 尾矿浆 康普顿散射 定量方法 

分 类 号：O657.34[理学—分析化学]