Abstract：Chemical composition of magnesite and dolomite is an important index for the detection of calcium-magnesium refractories. Magnesite and dolomite have large loss on ignition and are easily decomposed by heating. If the samples after burning are placed for long time or in improper way, it is very easy for them to absorb moisture and CO2 in the air, which leads to the deterioration and agglomeration, thus affecting the accuracy of determination results. Therefore, it is crucial to improve the accuracy of analytical methods by optimizing the measuring conditions reasonably.The contents of CaO, MgO, SiO2, Al2O3, Fe2O3 and P2O5 in magnesite and dolomite were determined by X-ray fluorescence spectrometry (XRF) with fusion sample preparation. The mass of sample after loss-on-ignition measurement was directly used as the amount of sample, which avoided the influence of moisture and CO2 in the air on sample mass to the maximum extent. Meanwhile, the operation steps were simplified and the detection time was shortened. The following experimental conditions were finally selected for sample preparation: Li2B4O7-LiBO2 (m∶m=67∶33) mixed flux was used; the dilution ratio between the burned sample to the flux was 1∶10; the ammonium iodide (NH4I) solution was used as the release agent; the melting temperature was 1050℃; the melting time was 15min. 12 certified reference materials were used to prepare the calibration curve, and the linear correlation coefficient was between 0.9997 and 0.9999. The certified reference materials of magnesite and dolomite were used for precision test. The relative standard deviations (RSD, n=10) of determination results of components were between 0.14% and 1.6%. The proposed method was applied for the determination of certified reference materials of magnesite and dolomite. The measurement results were basically consistent with the certified values. The relative errors (n=5) of components were between 0.15% and 5.88%.
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