Abstract：The accurate determination of conventional components in limestone has important significance for guiding metallurgical production.To address the challenges posed by the complicated acid dissolution process and the challenges in determining the silicon content,as well as issues with the crucible adhesion of molten material and limitations in the determination of sodium and potassium content due to the use of molten reagents in the alkali fusion method,the borate fusion sample preparation method of X-ray fluorescence spectrometry (XRF) was referenced.0.2 g of sample,1.0 g of Li2B4O7-LiBO2(m∶m=67∶33) mixture flux,and 8-10 drops of 300 g/L ammonium iodide solution were mixed in a platinum-gold crucible.After fusion at high temperature(1 000 ℃) for 10 min,the fully detachable glass beads could be formed.The glass beads were then dissolved with 10% nitric acid(V/V) by heating.The contents of eight elements,including Al,Fe,Mg,Mn,Si,Ti,K and Na,were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).Based on the intensity and interference of spectral lines,the analytical lines with simple background and few interfering elements were selected.The matrix matching method was used to eliminate the influence of matrix effects caused by the flux and the main component matrix.Under the selected working conditions,the linear correlation coefficients of the calibration curves for each element were all greater than 0.999,and the limits of detection were in range of 0.001-0.03 μg/g.The precision tests were conducted using two limestone samples according to the experimental method.The relative standard deviations(RSD,n=6) of determination results of Al,Fe,Mg,Mn,Si,Ti,K and Na(in oxides) were between 0.53% and 4.8%.Two certified reference materials(GBW03106a,YSBC28707a-2013) were determined,and the found results were consistent with the certified value/standard value,which could meet the requirements of GB/T 27417-2017 Guidelines for Confirmation and Validation of Chemical Analysis Methods for Conformity Assessment.
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