Determination of manganese, titanium, silicon and phosphorus in ferrophosphorus by inductively coupled plasma atomic emission spectrometry
YU Ya-hui1, 2, WANG Li-juan1, 2, WANG Su-mei1, 2 ZHANG Xiu-yan1, 2, ZHANG Hui-zhen1, 2
1. State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization, Baotou Research Institute of Rare Earths, Baotou 014030, China; 2. Rui Ke National Engineering Research Centre of Rare Earth Metallurge and Function Materials Co., Ltd., Baotou 014030, China
Abstract：During the determination of elemental contents in ferrophosphorus by chemical wet method, the samples are dissolved with acid. If hydrofluoric acid is not added, the sample dissolution is incomplete. If hydrofluoric acid is added, the silicon in sample will be converted to gaseous silicon tetrafluoride. Therefore, the sample must be melted with alkali for the simultaneous determination of manganese, titanium, silicon and phosphorus. The ferrophosphorus sample was melted with sodium hydroxide and sodium peroxide in experiments. After leaching with nitric acid, the contents of manganese, titanium, silicon and phosphorus were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The calibration curves were prepared by matrixing matching method. The linear correlation coefficients of calibration curves for testing elements were all 0.99998. Mn 257.610nm, Ti 334.941nm, Si 288.158nm and P 178.222nm were selected as the analytical lines. The limit of detection for manganese, titanium, silicon and phosphorus was 0.015%, 0.015%, 0.023% and 0.13%, respectively. Two ferrophosphorus certified reference materials and two ferrophosphorus samples were determined according to the experimental method. The relative standard deviations (RSD, n=11) of determination results were between 0.29% and 4.2%. The contents of manganese, titanium, silicon and phosphorus in ferrophosphorus were determined according to the experimental method and other methods (flame atomic absorption spectrometry (AAS) for manganese; X-ray fluorescence spectrometry (XRF) for titanium and phosphorus; silicon-molybdenum blue spectrophotometry for silicon). The results were consistent.
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