氢化物发生–原子荧光光谱法测定地球化学样品中硒总量影响因素探讨  

Discussion on the influencing factors of total selenium content in geochemical samples determined by hydride generation atomic fluorescence spectrometry

作　　者：蒲海钦 黄雪莲 PU Hai-Qin;HUANG Xue-Lian(Sichuan Xiye Testing Technology Co.,Ltd.,Chengdu 611730,China;Sichuan Yekan Design Group Testing Co.,Ltd.,Chengdu 610000,China)

机构地区：[1]四川省西冶检测科技有限公司,成都611730 [2]四川省冶堪设计集团检测有限公司,成都610000

出　　处：《实验室检测》2024年第10期91-94,共4页Laboratory Testing

摘　　要：目的提高原子荧光光谱法测定硒总量精密度和准确度。方法本文通过对氢化物发生–原子荧光光谱法测定地球化学样品中硒总量影响因素进行分析,探讨了样品消解、仪器自身清洁度、共存离子干扰三个方面影响因素。优化了样品消解过程,总结了样品测定过程中仪器应注意的问题以及判断和消除共存离子干扰的常用方法。结果通过13个国家一级标准物质验证了方法的可行性,方法检出限为0.006 mg/kg,低于DZ/T 0279.14—2016的检出限(0.01 mg/kg),测试标准物质的相对标准偏差为1.9%~7.9%,|Δlg C|均小于0.1,精密度、准确度满足DZ/T 0011—2015《地球化学普查规范(1∶50000)》中的要求。结论有效解决了原子荧光光谱法测定硒总量质量不稳定的情况,提高了精密度和准确度。Objective To improve the precision and accuracy of atomic fluorescence spectrometry for the determination of total selenium content.Methods This article analyzes the factors affecting the determination of total selenium in geochemical samples by hydride generation atomic fluorescence spectrometry,and explores three influencing factors:sample digestion,instrument cleanliness,and coexisting ion interference.Optimized the sample digestion process,summarized the issues that should be noted in the instrument during the sample determination process,as well as the common methods for identifying and eliminating coexisting ion interference.Results The feasibility of the method has been verified through 13 national first level standard reference materials,the detection limit of the method is 0.006 mg/kg,which is lower than the detection limit of DZ/T 0279.14-2016(0.01 mg/kg).The relative standard deviation of the test standard substance were 1.9%~7.9%,and|ΔlgC|were all less than 0.1.The precision and accuracy meet the requirements of DZ/T0011-2015 Geochemical Census Specification(1:50000).Conclusion Effectively solved the problem of unstable quality in the determination of total selenium by atomic fluorescence spectroscopy,and improved precision and accuracy.

关 键 词：氢化物发生–原子荧光光谱法 硒 影响因素 地球化学样品 

分 类 号：P59[天文地球—地球化学]