粉末压片制样-X射线荧光光谱法测定炉渣中9种组分

快速准确地测定炉渣中多种组分含量,既是冶炼生产工艺的要求,也是环境保护和冶金废弃物综合利用的要求。实验采用聚酯(PET)薄膜包裹粉末压片法制样,选取与待测样品粒度一致的炉渣标准样品与高纯物质按照不同的比例,配制成各组分含量从低到高具有一定梯度炉渣校准样品,对其拟合校准曲线,建立了X射线荧光光谱法(XRF)同时测定高炉渣、转炉渣、电炉渣或平炉渣中SiO₂、TFe、Al₂O₃、CaO、MgO、TiO₂、S、P₂O₅、TMn含量的快速分析方法。PET薄膜包裹压片制样,减少了粉尘污染,把对仪器损坏的几率降到了最低,而且可以防止压片暴露在空气中,增加压片保存时间。通过调整仪器分析参数,控制试样在粒度大小方面一致以及采用OXSAS软件自带的TL+方程同时进行谱线重叠干扰校正和基体效应校正,有效地克服了炉渣复杂体系中各元素谱线干扰与基体效应,实现了粉末压片制样-X射线荧光光谱法对炉渣各组分的测定。按照实验方法对高炉渣样品进行精密度试验,结果的相对标准偏差(RSD,n=10)为0.16%～2.1%。采用实验方法对高炉渣、转炉渣、电炉渣或平炉渣标准样品和实际样品进行测定,结果与认证值或熔融法测定值相吻合。

Determination of nine components in furnace slag by X-ray fluorescence spectrometry with pressed powder pellet

Rapid and accurate determination of multiple components in furnace slag is not only the requirement of smelting process,but also the requirement of environmental protection and comprehensive utilization of metallurgical waste.The sample was prepared by pressed powder pellet method with polyester (PET) thin film package in experiments.The calibration samples of furnace slag series with certain content gradient were synthesized using the certified reference materials (CRMs) of furnace slag and high purity substance with the same particle size as the sample to be tested.The calibration curves were fitted.Consequently, a rapid analysis method for the simultaneous determination of SiO₂,TFe,Al₂O₃,CaO,MgO,TiO₂,S,P₂O₅ and TMn in blast furnace slag,converter slag,electric furnace slag and open-hearth furnace slag by X-ray fluorescence spectrometry (XRF) was established.The sample preparation with PET package reduced the dust contamination,which deceased the probability of instrument damage to a minimum.Moreover,it could also prevent the sample from being exposed to the air,thus increasing the preservation time of the sample.The spectral overlapping interference and matrix effect were corrected by adjusting the parameters of instrument analysis, controlling the consistency of sample particle size,and using the TL+ equation of OXSAS software.The spectral overlapping interference and matrix effect in complex system of furnace slag were overcome effectively.The determination of components in furnace slag by XRF with pressed powder pellet was realized.The precision tests of blast furnace slag were performed according to the experimental method.The relative standard deviations (RSD, n=10) of measured results were between 0.16% and 2.1%.The proposed method was applied for the determination of components in CRM and actual samples of blast furnace slag,converter slag,electric furnace slag or open-hearth furnace slag.The found results were in good agreement with the certified values or those obtained by fusion methods.