摘要
采用X射线荧光光谱法同时测定硅酸盐和高铁高钛铝土矿中SiO_2、Al_2O_3、Fe_2O_3、TiO_2、K_2O、Na_2O、CaO、MgO、MnO、P_2O_5等主次组分。0.500 0g样品与5.000 0g Li_2B_4O_7-LiBO_2混合熔剂(质量比为67∶33)混匀后,加入脱模剂200g·L^(-1) NH_4Br溶液0.6mL,氧化剂500g·L^(-1) NH_4NO_3溶液1.0mL,在1 100℃下先预熔2min,再熔融8min制备熔片。选择土壤、水系沉积物、岩石、铝土矿、高岭土等国家一级标准物质以及人工合成的校准样品绘制校准曲线。方法应用于硅酸盐和铝土矿标准物质及实际样品的主次成分的测定,结果与标准物质认定值或实际样品化学法测定值一致,各组分测定结果的相对标准偏差(n=12)小于8.0%。
The major and minor components (SiO2, Al2O3, Fe2O3, TiO2, K2O, Na2O, CaO, MgO, MnO and P2O5) in silicate and bauxite with high content of iron and titanium were determined simultaneously by X-ray fluorescence spectrometry. The sample (0.500 0 g) was mixed well with lithium tetraborate-lithium metaborate (Li2B4O7-LiBO2, 5.000 0 g, mass ratio of 67:33), then 0.6 mL of 200 g·L^-1 NH4Br solution as releasing agent and 1.0 mL of 500 g·L^-1 NH4NO3 solution as oxidant were added, the mixture was pre-melt for 2 min and melt for 8 min at 1 100℃ to prepare the fuse piece. The calibration curves were plotted by using national level standard substances and artificial calibration samples of soil, stream sediment, rock, bauxite and kaolin ore. The proposed method was applied to the determination of the major and minor components in certified reference materials and real samples of silicate and bauxite, the results were consistent with the certified values and those obtained by chemical method, and RSDs (n=12) were less than 8.0%.
出处
《理化检验(化学分册)》
CAS
CSCD
北大核心
2018年第3期303-307,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
广西科学研究与技术开发计划项目(桂科能14123006-16)
关键词
X射线荧光光谱法
熔融制样
主次组分
硅酸盐
铝土矿
X-ray fluorescence spectrometry
fusion sample preparation
major and minor component
silicate
bauxite