熔融制样-X射线荧光光谱测定不锈钢渣中10种组分

采用玻璃片熔融方法制样,建立了X射线荧光光谱(XRF)分析不锈钢渣中氧化铝、二氧化硅、氧化钙、氧化镁、三氧化二铁、氧化锰、三氧化二铬、二氧化钛、氧化镍和五氧化二磷的快速检测方法。以四硼酸锂-偏硼酸锂(质量比1∶1)为熔剂,稀释比1∶24,在1 100 ℃下,静置5 min,摇摆20 min熔融,制得均匀不锈钢渣玻璃片。选用炉渣标准样品、三氧化二铬高纯试剂及镍标准溶液合成系列不锈钢渣校准样品,经X射线荧光光谱仪测定并绘制校准曲线,采用谱线重叠干扰校正系数和基体效应校正系数有效地消除了光谱干扰和基体效应。采用高纯氧化物和标准溶液配制不锈钢渣合成样品,采用实验方法对合成样品及生产样品进行分析,测定值与参考值或湿法测定值一致;精密度试验结果显示,各组分测定结果的相对标准偏差(RSD, n=9)为0.34%~9.4%。

Determination of ten components in stainless steel slag by X-ray fluorescence spectrometry

The sample was prepared by fusion method. The rapid determination method of aluminum oxide, silicon dioxide, calcium oxide, magnesium oxide, ferric oxide, manganese oxide, chromium oxide, titanium dioxide, nickel oxide and phosphorus pentoxide in stainless steel slag by X-ray fluorescence spectrometry (XRF) was established. The Li₂B₄O₇-LiBO₂ (mass ratio of 1∶1) was used as mixed flux. The dilution ratio was 1∶24. The uniform glass sheets of stainless steel slag were prepared by fusion at 1 100 ℃ for 5 min (standing) and 20 min (swing). The series stainless steel slag calibration samples were synthesized with furnace slag standard sample, Cr₂O₃ high-purity reagent and Ni standard solution. The synthetic samples were determined by XRF to plot the calibration curve. The spectral interference and matrix effect were effectively eliminated by using spectral +overlapping interference coefficient and theoretical alpha coefficient. The stainless steel slag synthetic samples(synthetized by high purity oxides and standard solution) and production samples were analyzed according to the experimental method. The found results were consistent with the reference values or those obtained by wet method. The precision test results indicated that the relative standard deviations (RSD, n=9) were between 0.34% and 9.4%.