首页|熔融制样-X射线荧光光谱法测定镁钙铁质振动料中主量成分

熔融制样-X射线荧光光谱法测定镁钙铁质振动料中主量成分

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为保证镁钙铁质振动料有良好的抗渣性和耐火度以及施工强度,需要严格控制其化学成分.采用Li2B4O7-LiBO2混合熔剂(m∶m=67∶33)熔融制样,以300 g/L NH4I溶液为脱模剂,在1 050 ℃下熔融15 min制得玻璃片,实现了X射线荧光光谱法(XRF)对镁钙铁质振动料中主量成分SiO2、Al2O3、Fe2O3、CaO、MgO的测定.参照镁钙铁质振动料的成分,用镁质耐火材料、石灰石、铝矾土等标准样品混合配制各主量成分含量具有一定梯度且能覆盖其含量跨度的校准样品系列绘制校准曲线,克服了镁钙铁质振动料没有标准样品的难题;以理论α系数法进行基体校正,消除了元素间的吸收和增强效应.以样品中各成分的含量为横坐标,其对应的荧光强度为纵坐标绘制校准曲线,各成分校准曲线精密度品质因子K<0.07,各成分的检出限在0.012%~0.057 9%之间.按照实验方法测定镁钙铁质振动料样品中的主量成分,各成分测定结果的相对标准偏差(RSD,n=12)在0.12%~2.6%之间.选取2个镁钙铁质振动料样品,按照实验方法测定其中SiO2、Al2O3、Fe2O3、CaO、MgO的含量,同时采用标准方法GB/T 5069-2015进行方法对比.结果表明,实验方法检测结果与标准方法的误差在标准方法GB/T 5069-2015规定的允许差范围之内.
Determination of major components in magnesium-calcium-iron oxide vibrating material by X-ray fluorescence spectrometry with fusion sample preparation
In order to ensure good slag resistance,refractoriness and construction strength of magnesium-calcium-iron oxide vibrating material,the chemical composition should be strictly controlled.The sample prepared at 1 050 ℃ for 15 min by fusion sample preparation with Li2B4O7-LiBO2(m∶m=67∶33)as mixed flux and 300 g/L NH4I solution as release agent.The determination of major components(including SiO2,Al2O3,Fe2O3,CaO and MgO)in magnesium-calcium-iron oxide vibrating material was realized by X-ray fluorescence spectrometry(XRF).On the basis of chemical composition of magnesium-calcium-iron oxide vibrating material,the calibration sample series,which had a certain gradient and a certain content span covering the content ranges of elements in the sample,were prepared by mixing the certified reference materials of magnesia refractory,limestone and bauxite to draw calibration curve.Thus,the problem that there were no certified reference materials for magnesium-calcium-iron oxide vibrating material was over-come.Theoretical α coefficient method was employed for matrix correction,eliminating the absorption en-hancement effect among elements.The calibration curves were drawn with the component contents as ab-scissa and their corresponding fluorescence intensity as ordinate.The precision quality factors of calibra-tion curves of components were K<0.07,and the limits of detection were in range of 0.012%-0.057 9%.The contents of major components in magnesium-calcium-iron oxide vibrating material samples were determined according to the proposed method.The relative standard deviations(RSD,n=12)of determination results were between 0.12%and 2.6%.The contents of SiO2,Al2O3,Fe2O3,CaO and MgO in 2 magnesium-cal-cium-iron oxide vibrating material samples were determined according to the proposed method.Mean-while,standard method of GB/T 5069-2015 was used for method comparison.The results showed that the errors between the proposed method and the standard method were within the allowable ranges specified in standard method of GB/T 5069-2015.

magnesium-calcium-iron oxide vibrating materialX-ray fluorescence spectrometry(XRF)fu-sion sample preparationmajor component

王志彪、李向威

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阳泉市综合检验检测中心,山西阳泉 045000

国家硅铝质耐火材料质量检验检测中心(山西),山西阳泉 045000

镁钙铁质振动料 X射线荧光光谱法(XRF) 熔融制样 主量成分

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(9)