Abstract：The flux crucible was formed using lithium tetraborate on wall to prevent platinum-gold crucible from corrosion by sample in oxidation fusion process. The pig iron sample was oxidized and dissolved by nitric acid (1+1). The residual liquid was evaporated at low temperature. Then lithium carbonate was added to prepare glass bead by fusion. The determination method of silicon, manganese and phosphorus in pig iron by X-ray fluorescence spectrometry (XRF) was established. The experiments showed that the prepared glass bead was tough, uniform and smooth under the following conditions: the mass ratio of lithium tetraborate, lithium carbonate and sample was 30:5:1; 3-5mL of 300g/L ammonium iodide solution was used as release reagent; the mixture was fused at 1050℃ for 20min. The calibration curves of silicon, manganese and phosphorus were established with certified reference materials of pig iron, manganese ore and iron ore. The linear correlation coefficient and regression accuracy of calibration curves were good. The limits of detection for silicon, manganese and phosphorus were between 1.32μg/g and 5.60μg/g. The precision test was investigated using one pig iron sample. The relative standard deviations (RSD, n=12) of determination results of elements were between 0.83% and 1.8%. The accuracy test results showed that the error between the determination values and certified values of certified reference material of pig iron was within the allowable range specified in national standard method.
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ZHAO Jing, LU Nü-ping, BAO Xi-bo. Determination of silicon, manganese and phosphorus in pig iron by X-ray fluorescence spectrometry with fusion sample preparation. , 2020, 40(7): 72-76.
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