粉末压片制样-X射线荧光光谱法测定精炼渣中8种主要组分  

Determination of 8 major components in refined slag by X-ray fluorescence spectrometry with pressed powder pellet sample preparation

作　　者：高延强[1] 祁巍 刘艳辉 常利民 赵留伟 GAO Yanqiang;QI Wei;LIU Yanhui;CHANG Limin;ZHAO Liuwei(Ningbo Iron and Steel Co.,Ltd.,Ningbo 315807,China)

机构地区：[1]宁波钢铁有限公司,浙江宁波315807

出　　处：《冶金分析》2025年第2期76-81,共6页Metallurgical Analysis

摘　　要：钢铁冶金企业精炼渣的化学组分一般采用X射线荧光光谱法(XRF)测定,虽然有国标方法可以参考,但分析速度不能满足冶炼炉前生产的要求。本方法采用粉末压片制样法,设定研磨时间为40 s,压片压力为40 MPa、保压时间为40 s;选择自制的8个精炼渣样品作为校准样品制作校准曲线,建立了粉末压片制样-X射线荧光光谱法测定精炼渣中二氧化硅、三氧化二铝、氧化钙、氧化镁、五氧化二磷、氧化锰、二氧化钛、铁等8种主要组分的方法。各组分的校准曲线线性相关系数均大于0.98。按照实验方法测定精炼渣样品中二氧化硅、三氧化二铝、氧化钙、氧化镁、五氧化二磷、氧化锰、二氧化钛、铁,结果的相对标准偏差(RSD,n=11)均小于0.06%。按照实验方法测定3个精炼渣样品,测定结果与化学湿法分析(其中二氧化硅采用高氯酸脱水重量-硅钼蓝光度法;三氧化二铝、氧化钙采用EDTA滴定法;氧化镁、五氧化二磷、氧化锰、二氧化钛、铁采用电感耦合等离子体原子发射光谱法)对比,结果相一致。The chemical composition of refined slag in iron and steel metallurgical enterprises is generally determined by X-ray fluorescence spectrometry(XRF).Although there are national standard methods for reference,the analysis speed cannot meet the production requirements in front of the smelting furnace.In this study,the sample was prepared by pressed powder pellet method.The grinding time was 40 s,the pressure was 40 MPa,and the holding time was 40 s.Eight self-made refined slag samples were selected as calibration samples to establish the calibration curve.The method for determination of eight major components in refined slag,including silicon dioxide,aluminum oxide,calcium oxide,magnesium oxide,phosphorus pentoxide,manganese oxide,titanium dioxide,and iron,was established by XRF with pressed powder pellet sample preparation.The linear correlation coefficients of calibration curves of components were all greater than 0.98.The contents of silicon dioxide,aluminum oxide,calcium oxide,magnesium oxide,phosphorus pentoxide,manganese oxide,titanium dioxide,and iron in the refined slag sample were determined according to the experimental method.The relative standard deviations(RSD,n=11)of determination results were all less than 0.06%.Three refined slag samples were determined according to the experimental method,and the measured results were consistent with those obtained by the chemical wet methods(where,the content of silicon dioxide was determined by perchloric acid dehydration gravimetry-silicon molybdenum blue spectrophotometry;the contents of aluminum oxide and calcium oxide were determined by EDTA titration;the contents of magnesium oxide,phosphorus pentoxide,manganese oxide,titanium dioxide,and iron were analyzed by inductively coupled plasma atomic emission spectrometry).

关 键 词：研磨 粉末压片制样 X射线荧光光谱法(XRF) 精炼渣 二氧化硅 三氧化二铝 氧化钙 氧化镁 五氧化二磷 氧化锰 二氧化钛 铁 

分 类 号：TF701.3[冶金工程—钢铁冶金] TF76[理学—分析化学] O657.34[理学—化学]