作者：刘攀^1,2, 李治亚¹, 杜米芳¹, 李景滨¹, 高灵清^1,3

作者单位：1. 中国船舶集团有限公司第七二五研究所（洛阳船舶材料研究所），河南 洛阳 471023;
2. 国家新材料生产应用示范平台（先进海工与高技术船舶材料），河南 洛阳 471023;
3. 河南省船舶及海工装备结构材料技术与应用重点实验室，河南 洛阳 471023

关键词：X射线荧光光谱法;波长色散;硅铝质矿物;玻璃熔铸法;烧失量

摘要：

硅铝质矿物是焊接药剂和耐火材料的重要原料，化学成分是评价其性能和质量的基本指标。研究硅铝质矿物熔融制片的样品粒径、熔融温度、熔剂、脱模剂等条件参数，优化X射线荧光光谱仪的最佳测量条件，通过烧失量校正模型消除高温熔融质量烧损引起的误差效应。采用系列粘土、高岭土、玻璃等标准物质，基于经验法构建校准曲线，建立X射线荧光光谱法快速测定硅铝质矿物中Al₂O₃、CaO、MgO、Na₂O、K₂O、TiO₂ 化学成分的方法。方法测定结果的相对标准偏差不大于3.5%，GBW 03102a标准物质的测定值与认定值相符，可用于硅铝质矿物质的快速检验。

Determination of aluminum, calcium, magnesium, sodium, potassium and titanium in silicon-aluminum mineral by wavelength dispersive X-ray fluorescence spectrometry with fusion sample preparation
LIU Pan^1,2, LI Zhiya¹, DU Mifang¹, LI Jingbin¹, GAO Lingqing^1,3
1. Luoyang Ship Material Research Institute, Luoyang 471023, China;
2. National New Material Production and Application Demonstration Platform (Advanced Marine Engineering and High-tech Ship Materials), Luoyang 471023, China;
3. Henan Key Laboratory of Technology and Application of Structural Materials for Ship and Marine Equipment, Luoyang 471023, China
Abstract: Silicon-aluminum mineral was the important raw material for welding flux and refractory materials, and the chemical composition was the basic index to evaluating its performance and quality. The working conditions, such as sample particle size, fusion temperature, flux, mold release agent, for the fusion preparation of silicon-aluminum mineral were studied. The best measurement conditions of X-ray fluorescence spectrometer were optimized. A loss-on-ignition correction model was established to eliminate the error effect caused by the high-temperature fusion mass burning loss. A series of certified reference materials, such as clay, kaolin, and glass, were used to construct the calibration curve, based on empirical methods. Then an X-ray fluorescence spectrometry method to quickly determine the chemical components of Al₂O₃, CaO, MgO, Na₂O, K₂O and TiO₂ in silicon-aluminum minerals was established, with the relative standard deviation not more than 3.5%. The GBW 03102a standard sample was determined, and the results were consistent with the certified values, which indicated that the experimental method could be used for the rapid analysis of silicon-aluminum mineral.
Keywords: X-ray fluorescence spectrometry;wavelength dispersive;silicon-aluminum sample;fused cast bead method;loss-on-ignition
2023, 49(3):79-83  收稿日期: 2021-04-05;收到修改稿日期: 2021-06-30
基金项目: 国家新材料生产应用示范平台建设项目（TC180A6MR/2）；七二五所科技创新项目（LW190602）
作者简介: 刘攀(1989-),男,江苏邳州市人,高级工程师,主要从事无机分析化学与冶金材料测试工作
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