Abstract：Chemical reagents such as strong acid and alkali are required during determination of chemical composition in ferromanganese alloy by traditional chemical wet method, which is time-consuming. Moreover, the operation skill is difficult to master. The application of X-ray fluorescence spectrometry (XRF) in the determination of ferromanganese alloy was investigated. A certain amount of sample and ferromanganese alloy oxidant were wrapped with filter paper in a ceramic crucible containing graphite powder. The sample was oxidized in a muffle furnace at 800 ℃. The oxidized samples were transferred to a platinum yellow crucible to prepare glass sheets for XRF analysis by a high-frequency melting machine with lithium tetraborate as the flux. As a result, the oxidization of samples outside the platinum-gold crucible was realized. It was effective to overcome the difficulties such as small volume of the platinum-gold crucible matched with the high-frequency melting machine and the preparation of flux crucible on the wall. Moreover, this method effectively solved the problem that the elements in ferromanganese alloy sample formed low temperature eutectic with platinum in fusion process, which would damage the platinum-gold crucible. Through conditional experiments, the fusion conditions were optimized as below: the sample mass was 0.200 0 g; the flux mass was 5.000 0 g; the sample fusion temperature was 1 050 ℃; the fusion time was 12 min. Consequently, a method for determination of silicon, manganese, and phosphorus in ferromanganese alloy was established by XRF with fusion sample preparation. The determination coefficients of calibration curves for silicon, manganese, and phosphorus were all not less than 0.999 8. The experimental method was applied to the daily inspection of ferromanganese alloy. The relative standard deviations (RSD, n=10) of determination results were all lower than 3%. The errors between the measurement values and certified values of certified reference materials could be controlled within the permissible range of chemical analysis method in national standard.
闫丽. 熔融制样-X射线荧光光谱法测定锰铁合金中硅锰磷[J]. 冶金分析, 2022, 42(6): 45-50.
YAN Li. Determination of silicon, manganese and phosphorus in ferromanganese alloy by X-ray fluorescence spectrometry with fusion sample preparation. , 2022, 42(6): 45-50.
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