Guo Yanqing, Lu Fei, Fan Xin
The analytical capability of X-ray fluorescence (XRF) spectrometry under vacuum environment for the determination of carbon in cast iron, high-chromium cast iron, medium-low alloy steel, and stainless steel with varying carbon contents was investigated in this study. The instrumental measurement conditions, including tube voltage, tube current, analysis angle, counting time, pulse height distribution (PHD), window width, and background subtraction, were optimized. When the sample was treated using a milling machine, a cutter head rotation speed of 600 r/min and a milling forward speed of 300 mm/min could yield consistent and fine-textured sample surfaces, thus ensuring the accuracy of results. In addition, the samples should be prepared and analyzed promptly. If the samples were stored for too long, their surfaces must be reprepared prior to analysis. Under the optimized experimental conditions, an analytical method for determining carbon in cast iron, high-chromium cast iron, medium-low alloy steel, and stainless steel by XRF was established. The limits of detection for carbon in cast iron, high-chromium cast iron, medium-low alloy steel, and stainless steel were 0.030%, 0.023%, 0.015%, and 0.015% (mass fraction, similarly hereinafter), respectively. The precision and trueness of carbon analysis results were examined. The relative standard deviation (RSD) of carbon determination results in cast iron, high-chromium cast iron, and medium-low alloy steel samples ranged from 0.64% to 1.9%. For stainless steel samples, as the carbon content decreased, the RSD increased and the analytical precision decreased. The trueness verification results indicated that when the carbon content was higher than 0.15%, the XRF results were in good agreement with the certified values of standard reference materials or the results obtained by high-frequency induction furnace combustion followed by infrared absorption spectrometry. In iron and steel smelting, for the samples with a carbon content greater than 0.15%, a simultaneous detection of carbon content during analysis could be attempted to improve the analytical efficiency of XRF in steelmaking processes.