粉末灼烧压片-X射线荧光光谱法测定石灰类材料中组分基体干扰的消除方法研究

通过石灰石标准样品高温灼烧后绘制校准曲线，解决了绘制校准曲线用活性类石灰无标准样品，又难同时准备足够多且有梯度生产样品等难题；烧结用石灰样品经高温灼烧后压片制样，大大减小了石灰样品基体干扰并完全消除粒度效应，从而实现粉末压片-X射线荧光光谱法对石灰石、活性石灰、生石灰中氧化钙、氧化镁和二氧化硅含量的测定。氧化钙、氧化镁和二氧化硅校准曲线的相关系数均大于0.999。对同一活性石灰样品进行精密度考察，3种组分测定结果的相对标准偏差(RSD，n=11)在0.086%～2.3%范围内。对生石灰、活性石灰炼铁烧结工序生产样品进行分析，测定值与熔融制样-X射线荧光光谱法的测定值一致；对石灰石标准样品进行分析，测定值与校正后的认定值相吻合。

Study on the elimination method of matrix interference during the determination of components in lime materials by X-ray fluorescence spectrometry with pressed powder pellet after ignition

The calibration curve was plotted using standard sample of lime after high temperature ignition, solving the problems such as lack of certified reference materials for active lime, difficulty to prepare enough production sample with gradient at the same time. The sample was prepared by pressing using sintering lime samples after high temperature ignition. The matrix interference was greatly reduced, and the granularity effect was completely eliminated. The content of calcium oxide, magnesium oxide and silicon dioxide in limestone, active lime and quick lime was determined by X-ray fluorescence spectrometry with pressed powder pellet. The correlation coefficients of calibration curves of calcium oxide, magnesium oxide and silicon dioxide were all higher than 0.999. The precision test was conducted using one active lime sample. The relative standard deviations (RSD, n=11) of three components were between 0.086% and 2.3%. The production samples of quick lime and active lime in sintering process of iron-making were analyzed. The found results were consistent with those obtained by X-ray fluorescence spectrometry with fusion sample preparation. The standard sample of limestone was also analyzed, and the found results were consistent with the certified values after correction.