Citation:
YAN Zi-Xin, QU Jing-Kui, YU Zhi-Hui, SONG Jing, WEI Guang-Ye. Multi-spectral Fitting-Determination of Trace Cobalt in High Purity Nickel by Inductively Coupled Plasma Atomic Emission Spectrometry[J]. Chinese Journal of Analytical Chemistry,
;2019, 47(3): 423-428.
doi:
10.19756/j.issn.0253-3820.181622
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By comparing the methods of matrix matching and standard addition and multi-spectral fitting (MSF) for elimination of interference, an analytical method for the determination of trace cobalt in high purity nickel by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The optimum parameters of the instrument were determined as follows:RF power of 1350 W, atomizer velocity of 0.5 L/min, observation distance of 15 mm, and peristaltic pump speed of 1.0 mL/min. Three calibration methods, matrix matching, standard addition and MSF, were used to determine the standard addition of pure nickel solution. When the standard addition concentrations were 0.10 and 0.20 mg/L, and nickel concentration was 5 g/L, the three methods all could get good recovery. The linear correlation coefficients were all greater than 0.9996, the recoveries were 95.0%-102.0%, and the RSDs were 2.1%-4.6%. The linear range of MSF method was the best (0.02-0.5 mg/L) and the detection limit was the lowest (0.002 mg/L). When the standard addition concentrations of nickel were 0.02 and 0.06 mg/L and the nickel concentration was 15 g/L, the results showed that only the MSF method could get accurate results with linear correlation coefficient of 0.9999, linear range of 0.02-0.1 mg/L, detection limit of 0.002 mg/L, recoveries of 95.0%-105.0%, and RSDs of 3.9%-4.6%. The MSF method was used to test the actual samples. The analytical results were 0.000154%, which was consistent with the GD-MS method. The RSD was 2.3%. The accuracy and precision of the method were further verified. MSF method is not only strong in anti-interference, simple in operation, economical and practical, but also has high precision, low detection limit. The lower limit of detection (0.0001%) and detection range are superior to the national standard atomic absorption spectrometry (0.001%). It provides an important methodological method for the determination of trace impurities in high-purity samples.
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