Determination of nickel, copper, iron, tin, phosphorus and sulfur in nickel-copper-iron alloy by X-ray fluorescence spectrometry with high-frequency fusion sample preparation
SONG Zu-feng1,2, LU Xiang-dong3, WANG Zhong-le1, SUN Zhi-peng1 FU Wan-yun1, WANG Chen-weng4
1. Technology Center of Maanshan Iron & Steel Co., Ltd., Maanshan 243000, China; 2. Key Parts of Rail Transit Technology Innovation Center of Anhui Province, Maanshan 243000, China; 3. Jiangsu Yonggang Group Co., Ltd., Zhangjiagang 215628, China; 4. Lirun Electromechanical Equipments Co., Ltd., Shanghai 200082, China
Abstract：Nickel-copper-iron alloy belongs to irregular sample and only one sample could be prepared in single sample preparation by centrifugal casting method. A multi-functional melting furnace was used to prepare the mushroom-shaped block samples by high-frequency fusion casting. The determination of nickel, copper, iron, tin, phosphorus and sulfur in nickel-copper-iron alloy by X-ray fluorescence spectrometry (XRF) was realized. The working parameters of the multi-functional melting furnace were optimized. The program-controlled step heating was used, and the heating and heat preservation of the 5th stage were adopted to melt the samples. The optimal sample preparation process was obtained. The experimental results showed that when the maximum target power was 12.75kW, the heating time of each stage was 10s, and the entire melting time was 10min, the chemical composition of each testing element in the sample with fusion preparation had good homogeneity in the depth direction of 0-0.50mm. Moreover, the repeatability of sample was good under the same melting conditions. The calibration curve was established using spectral standard samples of nickel alloy, nickel-chromium alloy and high-alloy steel and chemically-defined internal control samples of nickel-copper-iron alloy with certain concentration gradients. The linear correlation coefficients of all testing elements were higher than 0.999. The limits of detection were between 12.35μg/g and 42.21μg/g. The relative standard deviations (RSD, n=10) of determination results of ten block samples were between 0.15% and 1.9%. The proposed method was applied to the determination of nickel-copper-iron alloy actual samples. The found results were in good agreement with those obtained by standard method, which could meet the testing requirement of routine analysis.
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SONG Zu-feng, LU Xiang-dong, WANG Zhong-le, SUN Zhi-peng FU Wan-yun, WANG Chen-weng. Determination of nickel, copper, iron, tin, phosphorus and sulfur in nickel-copper-iron alloy by X-ray fluorescence spectrometry with high-frequency fusion sample preparation. , 2020, 40(9): 31-37.
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