Determination of multi-elements in ferroboron by X-ray fluorescence spectrometry with powder pellet preparation
Accurate and rapid determination of boron and impurities in ferroboron is of great importance for the scientific guidance of ironmaking and steelmaking production as well as ensuring the quality of high val-ue-added steel.In this study,the sample was prepared by powder pressed pellet.The calibration sample series,which had a certain gradient and a certain content span covering the content ranges of elements in the sample,were prepared with 2 ferroboron certified reference materials and ferroboron samples deter-mined by national standard method to overcome the matrix effect.Thus,the determination of B,Al,Si,P,S,Ti and Mn in ferroboron was realized by X-ray fluorescence spectrometry(XRF).The sample prepa-ration conditions were optimized:1.50 g of sample with particle size of 53 μm(screened with 280 mesh)was edged with boric acid and then pressed at 44 MPa for 40 s.The matrix effect of boron was corrected by concentration correction with empirical coefficient method.The limits of detection were listed as below:0.085％for B,0.000 99％for Al,0.001 9％for Si,0.000 72％for P,0.000 41％for S,0.003 4％for Ti,and 0.003 9％for Mn.The proposed method was applied for the determination of 6 different pellets which were parallelly prepared with ferroboron samples.The relative standard deviations(RSD)of deter-mination results of elements were all less than 2.0％.The ferroboron samples were determined according to the proposed method,and the results were basically consistent with those obtained by other methods:B was determined by alkalimetry in GB/T 3653.1-1988;Al was determined by EDTA titration method in GB/T 3653.4-1988;Si was determined by perchloric acid dehydration gravimetry in GB/T 3653.3-1988;P was determined by antimony phosphomolybdenum blue spectrophotometry in GB/T 3653.6-1988;S was determined by infrared absorption method in GB/T 3653.7-2020;Ti and Mn were determined by inductive-ly coupled plasma-atomic emission spectrometry in GB/T 6730.63-2006.
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