Determination of 5 components in ladle nozzle flocculation by X-ray fluorescence spectrometry with fusion sample preparation
KANG Dehua1,2, YANG Jie2, HU Zhongxin2, DENG Junhua1,2, WANG Yiling1,2
1. State Key Laboratory of Metal Material for Marine Equipment and Application,Anshan 114009,China; 2. Iron & Steel Research Institute of Ansteel Group,Anshan 114009,China
Abstract：The phenomenon of flocculation at ladle nozzle often occurs during the pouring of certain steel grades in steel-making plants. The semiquantitative analysis by X-ray fluorescence spectrometry (XRF) indicated that the nozzle flocculation was mainly composed of Al2O3, CaO, SiO2, MgO and Fe. The chemical composition analysis usually adopts titration, spectrophotometry or atomic absorption spectrometry (AAS), and so on. However, these methods have some disadvantages such as complex operation and long procedures. The sample was prepared by fusion method with Li2B4O7-LiBO2 mixed flux (m:m＝67:33) and dilution ratio of 1:12.5, and 0.15 g of NH4I was added as release reagent. The mineral effect of sample was eliminated, and the influence of matrix effect was reduced. The certified reference materials such as bauxite, mullite, pyroxene, and blast furnace slag, which have the similar matrix with ladle nozzle flocculation were selected. Then the calibration curves were drawn with these certified reference materials and the calibration samples by mixing these certified reference materials in different proportions, solving the problem that there was no certified reference material of ladle nozzle flocculation. The absorption enhancement effect of spectral intensity caused by the matrix was corrected with empirical coefficient method. The correlation coefficients of calibration curves were all greater than 0.998 9. The analysis method for simultaneous determination of Al2O3, CaO, SiO2, MgO, and total iron (TFe) in ladle nozzle flocculation was established by XRF with fusion sample preparation. The limits of detection were between 0.009% and 0.014%. One ladle nozzle flocculent sample was determined according to the proposed method. The relative standard deviations (RSD, n=10) of determination results were all less than 3.0%. Two ladle nozzle flocculent samples were determined respectively by the proposed method and GB/T 5069-2015, and the differences of the two above methods were all less than the tolerance of GB/T 5069-2015.
亢德华, 杨洁, 胡忠新, 邓军华, 王一凌. 熔融制样-X射线荧光光谱法测定钢包水口絮流物中5种组分[J]. 冶金分析, 2024, 44(6): 64-68.
KANG Dehua, YANG Jie, HU Zhongxin, DENG Junhua, WANG Yiling. Determination of 5 components in ladle nozzle flocculation by X-ray fluorescence spectrometry with fusion sample preparation. , 2024, 44(6): 64-68.
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