X射线荧光光谱法同时测定泥岩中26种组分  

Simultaneous Determination of 26 Components in Mudstone by X-ray Fluorescence Spectrometry

作　　者：王顺祥 王睿 帅林阳 王立华 魏巍 卜道露 丁洋 WANG Shunxiang;WANG Rui;SHUAI Linyang;WANG Lihua;WEI Wei;BU Daolu;DING Yang(Civil-Military Integration Center of China Geological Survey,Chengdu,Sichuan 611732,China)

机构地区：[1]中国地质调查局军民融合地质调查中心,成都611732

出　　处：《中国无机分析化学》2025年第4期506-514,共9页Chinese Journal of Inorganic Analytical Chemistry

基　　金：中国地质调查局地质调查项目(DD20243098);甘肃省文县阳山金矿资源基地综合调查项目(DD20220971)。

摘　　要：泥岩样品分析对研究古气候与古环境有着重要的作用,但是在日常分析中主次痕量元素很难用同一种方法进行测定。因此,提出了X射线荧光光谱法同时测定泥岩样品中26种组分(Na_(2)O、MgO、Al_(2)O_(3)、SiO_(2)、K_(2)O、CaO、TFe_(2)O_(3)、Ba、Cl、Co、Cr、Cu、Ga、Mn、Ni、Nb、P、Pb、Rb、Sr、Ti、V、Y、Zn、Zr、Hf)的方法。泥岩样品经粉碎棒磨(粒径小于74μm),再经60℃烘干,烘干后于多头混样机再研磨15 min,减少了粒度效应,试样保压在3 500 MPa的压力下15 s,压制的圆片光滑稳定。针对泥岩样品主要包含黏土矿物、沉积物、岩石等物质,通过选用112种岩石、沉积物和土壤国家一级标准物质拟合工作曲线进行测定,对测量条件进行了优化,利用SuperQ 5.0软件的综合数学校正公式进行基体效应和重叠干扰元素校正,选择页岩GBW07107和泥质灰岩GBW07108对方法准确度和精密度进行了考察,26种组分的准确度和精密度均比较良好,同时对吐哈盆地中侏罗统西山窑组3个泥岩样品进行了方法对比验证,结果表明,X射线荧光光谱法与电感耦合等离子体质谱(ICP-MS)、电感耦合等离子体原子发射光谱(ICP-AES)法测定结果基本一致,能满足日常分析测试需求。The analysis of mudstone samples plays an important role in the study of paleoclimate and paleoenvironment.However,it is difficult to use the same method to determine the major,minor and trace elements of mudstone samples in daily analysis.Therefore,a method for simultaneous determination of 26 components(Na_(2)O,MgO,Al_(2)O_(3),SiO_(2),K_(2)O,CaO,TFe_(2)O_(3),Ba,Cl,Co,Cr,Cu,Ga,Mn,Ni,Nb,P,Pb,Rb,Sr,Ti,V,Y,Zn,Zr,Hf)in mudstone samples by X-ray fluorescence spectrometry was proposed.The mudstone samples were ground by grinding rod(particle size less than 74μm),then dried at 60℃.After drying,the samples were ground again for 15 min on a multi-head mixing machine,which reduced the particle size effect.The samples were kept under a pressure of 3500 MPa for 15 s,which made the pressed discs smooth and stable.As the mudstone samples mainly contain clay minerals,sediments,rocks and other substances,112 kinds of national reference materials of rock,sediment and soil were selected to determine the fitting working curve.The measurement conditions were optimized,and the matrix effect and overlapping interference elements were corrected by using the comprehensive mathematical correction formula of SuperQ5.0 software.The accuracy and precision of the method were investigated by selecting GBW07107 and GBW07108,and the accuracy and precision of 26 components were relatively good.At the same time,three mudstone samples from the Xishanyao Formation of Middle Jurassic in Tuha Basin were compared and verified,and the results showed that the method was basically consistent with the determination results of ICP-MS and ICP-AES.The method can meet the needs of daily analysis and testing.

关 键 词：X射线荧光光谱法 泥岩 谱线干扰重叠 基体效应 

分 类 号：O657.34[理学—分析化学]