熔融制样-X射线荧光光谱法测定硅酸盐样品中主量元素

摘要

The glass fuse piece was prepared by a melting method with lithium tetraborate and lithium metaborate (mass ratio of 67 ∶ 33) as fusing reagent,ammonium bromide as release agent and ammonium nitrate as oxidant.Calibration curve fitting was performed with Chinese National Standard Materials of soil,rock and stream sediment,the matrix effect was corrected by experienced coefficients and all of the linear correlation coefficients were up to 0.999.Ten major components including SiO2,Al2O3,TFe2O3,TiO2,K2O,Na2O,CaO,MgO,MnO and P2O5 were simultaneously determinated by Japanese science Primus Ⅱ X-ray fluores cence spectrometry,the proposed method was applied to the determination of certified reference material and silicate samples,the results were consistent with the certified values and those obtained by chemical method.The relative standard deviation(RSD,n =12) of components was less than 5％,the accuracy and precision reached standard specification requirements of geology and mineral resources industry.The method was sim ple,rapid,accurate,efficient and environmentally friendly,which can satisfy the requirements of rapid analysis major elements in silicate sample.Experimental results demonstrated that it was feasible to use X-ray fluorescence spectrometry to analyze the major components content in silicate samples.%采用熔融制样,以四硼酸锂-偏硼酸锂(质量比为67∶33)作熔剂,溴化铵作脱模剂,硝酸铵作氧化剂制备玻璃熔片.选用土壤、岩石、水系沉积物等国家标准物质拟合校准曲线,用经验系数法校正元素间的基体效应,各组分的线性相关系数均达到了0.999以上.使用日本理学ZSX PrimusⅡ型光谱仪对样品中SiO2、Al2O3、TFe2O3、TiO2、K2O、Na2O、CaO、MgO、MnO、P2O5等10种组分进行同时测定,分析结果与标准物质认定值或化学方法结果相符,相对标准偏差(RSD,n=12)小于5％,准确度和精密度均已达到地质矿产行业标准规范要求.方法简便、快速、准确、高效且绿色环保,满足了硅酸盐样品中主量元素快速分析测试的需求.实验表明,利用X射线荧光光谱法对硅酸盐主要成分含量进行同时分析是可行的.