Determination of fluorine in fluorine-containing cerium-based rare earth polishing powder by alkali fusion-EDTA titration
ZHANG Hong1, 2, WANG Su-mei1, 2, WANG Dan1, 2
1. Baotou Research Institute of Rare Earths, Baotou 014030, China; 2. State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization, Baotou 014030, China
Abstract:The content of fluorine in fluorine-containing cerium-based rare earth polishing powder is 1%-8% (mass fraction). During the sample treatment by steam distillation, the operation is cumbersome and difficult to master. The sample was melted with sodium hydroxide-sodium peroxide mixed flux at high temperature (750℃) for 10min followed by water leaching and filtration. The fluorine in sample was totally transferred to filtrate, realizing the separation with rare earths. The pH of solution was adjusted to about 2 to precipitate fluorine with excessive lanthanum. After boiling for 1-2min, the residual lanthanum was titrated with EDTA in hexamethylenetetramine-hydrochloric acid buffer system. The content of fluorine in sample was indirectly determined. The proposed method was applied for the determination of fluorine in fluorine-containing cerium-based rare earth polishing powder. The relative standard deviations (RSD, n=11) of measurement results were between 0.88% and 2.9%. The content of fluorine in standard sample of polishing powder (GSB04-3426-2017) was determined according to the experimental method, and the found results were consistent with the certified values. The contents of fluorine in standard sample (GSB04-3426-2017) and actual sample of fluorine-containing cerium-based rare earth polishing powder were determined according to the experimental method and the method in national standard GB/T 20166.2-2006. The determination results of two methods were consistent.
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