Abstract:During the analysis of high content silicon [w(Si)≥3.0%] by spark discharge atomic emission spectrometer, the elemental content was beyond the linear range of calibration curve, leading to the lower determination results. The standard samples of middle-low alloy steel and silicon steel were added in experiments to improve and expand the calibration curve of silicon. The interference of coexisting elements was corrected. The analysis range of silicon was broadened. The upper limit of mass fraction increased from 3.14% to 4.16%, and the linear correlation coefficient was up to 0.99965. After extension of calibration curve, the standardization sample was reselected for the drift correction. The intensity ratio of calibration curve was expanded from 9.41 to 11.01. Two samples with expanded silicon content [w(Si)≥3.0%] were used for precision test. The relative standard deviation (RSD, n=10) was 0.43% and 0.50%, respectively. Eight samples with different silicon contents were compared. It was found that the determination results by expanded calibration curves were more consistent with the certified values. Meanwhile, the statistical process control (SPC) chart was within the controlled state. Therefore, the modified and expanded calibration curve could meet the process control and analysis requirements of products.
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