Abstract：In order to solve the corrosion problem of platinum crucible caused by reducing substances in nickel-chromium pig iron samples during high temperature melting, a one-step melting method was developed to prepare nickel-chromium pig iron glass sheet. 0.1 g of sample was weighed. The flux was added by 5.0 g of lithium tetraborate, 2.0 g of lithium metaborate, and 1.5 g of lithium tetraborate covering method. 1.0 g of lithium carbonate was used as oxidant. After the sample was melted at 700 ℃ for 10 min and 850 ℃ for 10 min, a smooth, flat and uniform glass sheet was obtained with 500 g/L lithium bromide solution as release agent. The production samples with a certain content span and a certain content gradient, which were determined by national standard methods, were used as calibration sample series to draw calibration curves. The overlapping corrections of iron and silicon were conducted with chromium, respectively. The matrix corrections of spectral lines of nickel, chromium and phosphorus were not required. The prepared glass sheet was determined by X-ray fluorescence spectrometry (XRF). Thus, a method for determination of total iron(TFe), nickel, phosphorus, chromium and silicon in nickel-chromium pig iron was established. The contents of TFe, nickel, phosphorus, chromium and silicon in five nickel-chromium pig iron samples were determined according to the proposed method, and the relative standard deviations (RSD, n=11) were between 0.13% and 1.3%. The proposed method was compared with national standard methods and inductively coupled plasma atomic emission spectrometry (ICP-AES). It was found that the results were basically consistent. In the proposed method, the procedures of pre-oxidation and melting were integrated by a fully automatic melting furnace for sample preparation. The complicated wall hanging operation was not required. Moreover, it could effectively protect the crucible from corrosion.
刘云利, 曾垚. 熔融制样-X射线荧光光谱测定镍铬生铁中主次成分[J]. 冶金分析, 2024, 44(6): 57-63.
LIU Yunli, ZENG Yao. Determination of major and minor elements in nickel-chromium pig iron by X-ray fluorescence spectrometry with fusion sample preparation. , 2024, 44(6): 57-63.
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