Determination of six components in microcrystalline cast stone by X-ray fluorescence spectrometry with fusion sample preparation
KANG De-hua1,2, YU Yuan-jun1,2, DENG Jun-hua2, WANG Yi-ling2, LI Ying2
1. State Key Laboratory of Marine Equipment Made of Metal Material and Application, Anshan 114009, China; 2. Iron & Steel Research Institute of Ansteel Group, Anshan 114009, China;
Abstract：The production of microcrystalline cast stone from industrial residues (blast furnace slag, steel slag, copper slag, chromium slag, ferroalloy slag, etc) as main raw materials has great benefits. At present, the major components in microcrystalline cast stone (SiO2, Al2O3, CaO, MgO, TFe and TiO2) are usually analyzed by chemical wet method, which has some disadvantages such as relatively complicated operation and long analysis procedures. The sample was prepared by fusion method using Li2B4O7-LiBO2 mixed flux (m∶m=67∶33). The mass ratio between the sample and flux was 1∶12.5. The pre-oxidation by oxidant was not required. 0.15g of NH4I was added as the release agent. The mineral structure effect of sample was eliminated and the influence of matrix effect was reduced. Thus the simultaneous determination of SiO2, Al2O3, CaO, MgO, TFe and TiO2 contents in microcrystalline cast iron by X-ray fluorescence spectrometry (XRF) with fusion sample preparation was realized. The calibration sample was artificially synthesized using the national-grade and industry-grade certified reference materials of converter slag, blast furnace slag, Guye chamotte and bauxite, which had similar matrix to microcrystalline cast stone, to prepare the calibration curve. The problem that there was no standard material of microcrystalline cast stone was solved. The matrix effect and spectral interference were eliminated by the mathematical regression method, the fundamental parameter method and the theoretical influence coefficient method. The correlation coefficients of calibration curves were all higher than 0.999. One microcrystalline cast stone sample was determined for the precision test. The relative standard deviation (RSD, n=10) of determination results of six components were all less than 5.0%. The correctness verification results indicated that the determination results of proposed method were in good agreement with those obtained by other methods.
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KANG De-hua, YU Yuan-jun, DENG Jun-hua, WANG Yi-ling, LI Ying. Determination of six components in microcrystalline cast stone by X-ray fluorescence spectrometry with fusion sample preparation. , 2018, 38(8): 32-36.
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