熔融制样-X射线荧光光谱法测定铝锆碳、锆碳质耐火材料中的主次成分

Determination of major and minor components in alumina-zirconia-carbon or zirconia-carbon refractories by X-ray fluorescence spectrometry with fusion sample preparation technique

建立了混合氧化剂预氧化后硼酸盐熔融制样-X射线荧光光谱法测定铝锆碳、锆碳质耐火材料中ZrO_2、HfO_2、Al_2O_3、SiO_2、CaO、MgO、Fe_2O_3、TiO_2等组分的方法,讨论了混合氧化剂配比、氧化时间、灼烧减量、熔剂及稀释比等因素对制样及分析结果的影响。结果表明,按照Na_2O_2 4倍于试样量、NaNO_3 2倍于试样量配制混合氧化剂,氧化时间90min,碳的去除率最高;使用四硼酸锂偏硼酸锂混合熔剂(质量比67∶33),稀释比30∶1,可熔制出满足要求的熔片;曲线标样与试样间灼烧减量的差异给试样分析结果带来的偏差可以通过灼烧减量计算予以校正。经验证,该方法分析精密度较好,各元素9次平行分析结果的相对标准偏差均在3.25%以下,与化学湿法分析结果的一致性较好。

A X-ray fluorescence spectrometry method was established for determination of ZrO_2、HfO_2、Al_2O_3、SiO_2、CaO、MgO、Fe_2O_3、TiO_2 in Alumina-Zirconia-Carbon or Zirconia-Carbon refractories with fusion sample preparation technique.A preoxidation process with mixed oxidant was used before fusion.The effects of oxidation time,proportion of mixed oxidant,flux,dilution ratio,LOI on sampling and analysis results were discussed.The results showed that when the mass ratio of Na_2O_2 to sample was 4,the mass of NaNO_3 was two times as sample,the oxidation time was 90 minutes,the carbon removal rate of sample was highest.When the mass ratio of mixed flux（mass ratio,Li_2B_4O_7∶LiBO_2=67∶33）to sample was 30∶1,the glass bead was much more better.Moreover,it proved that the loss on ignition would lead to deviation of analysis results in this paper,and the deviation could be corrected by calculation method with LOI.The test showed that this method presented good precision,the relative standard deviation of all elements were lower than 3.25%,and the results determined by this method were according well with chemical results.