摘要
以标准物质及标准物质与基准试剂氧化镁、氧化钙人工混合配制标样的方法建立标准工作曲线,探讨了各元素测定的仪器条件、标准工作曲线的配制方案、理论α系数校正基体效应,建立了用X射线荧光光谱(XRF)法测定绿泥石中镁、铝、硅、磷、钾、钙、钛、铁8种元素含量的快速分析方法。通过熔剂和脱模剂的选取,最终得出最佳熔样条件为采用8.0 g四硼酸锂和偏硼酸锂混合熔剂(质量比67∶33)+0.8 g样品,并添加溴化锂作为脱模剂,熔样温度1100℃,熔样时间10 min。与传统的重量法、容量法、分光光度法相比,X射线荧光光谱法具有能同时测定多种元素,并且具有测量范围广、精密度及准确度高、分析速度快等特点,方法的相对标准偏差(n=12)均小于5.6%,实际绿泥石样品测定结果与化学法一致,硅酸盐标准物质GBW03131滑石、GBW07103花岗岩、GBW07301a水系沉淀物、GBW07309水系沉淀物、GBW07107页岩测定结果均满足不确定度要求。X-射线荧光光谱熔片法成本低、流程短、测定结果可靠,为绿泥石成分检测提供了一种快速的分析方法。
A rapid method for the determination of magnesium,aluminum,silicon,phosphorus,potassium,calcium,titanium and iron in chlorite by X-ray fluorescence spectrometry(XRF)was established.The standard working curve was established by manually mixing standard materials and reference reagents such as magnesium oxide and calcium oxide.The instrument conditions for the determination of each element,the formulation scheme of standard working curve,the matrix effect of theoreticalαcoefficient correction,and the selection of flux and release agents were discussed.The optimum melting conditions were obtained as follows:8.0 g mixed flux of lithium tetraborate with lithium metaborate(mass ratio 67∶33)+0.8 g sample and adding lithium bromide as release agent,melting temperature 1100℃,melting time 10 min.Compared with the traditional gravimetric,volumetric and spectrophotometer methods,the X-ray fluorescence spectrometry has the advantages of simultaneous determination of multiple elements,wide measurement range,high precision and accuracy,and fast analysis speed.The relative standard deviation(RSD)of this method(n=12)was less than 5.6%.The results of practical chlorite samples determination were consistent with those of chemical method,and certificated reference materials of silicate such as talc(GBW03131),granite(GBW07103),sediment of water series(GBW07301A),sediment of water series(GBW07309)and shale(GBW07107)all meet the requirements of uncertainty.It showed that the method has good precision and accuracy.X-ray fluorescence spectrometry method has the advantages of low cost,short process and reliable determination results,which provides a fast analytical method for determining the composition of chlorite.
作者
冯丽丽
张庆建
管嵩
赵雷
郭志东
FENG Lili;ZHANG Qingjian;GUAN Song;ZHAO Lei;GUO Zhidong(Technical Center of Qingdao Customs,Qingdao,Shandong 266500,China;Qingdao University of Technology,Qingdao,Shandong 266520,China;Shandong university of Technology,Zibo,Shandong 255049,China)
出处
《中国无机分析化学》
北大核心
2024年第3期312-317,共6页
Chinese Journal of Inorganic Analytical Chemistry
基金
国家重点研发计划项目(2022YFC3002402)。
关键词
绿泥石
X射线荧光光谱
主次元素测定
chlorite
X-ray fluorescence spectrum
determination of primary and secondary elements
