Determination of rare earth elements in rare earth-aluminum intermediate alloy by X-ray fluorescence spectrometry with fusion sample preparation
REN Xu-dong1,2,3, NIE Cheng-hong1,2,3, WANG Zhen-jiang1,2,3, WU Wen-qi1,2,3, LIU Dan-na1,2,3
1. State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization, Baotou Research Institute of Rare Earths, Baotou 014030, China; 2. National Engineering Research Centre of Rare Earth Metallurgy and Functional Materials, Baotou 014030, China; 3. Baotou Research Institute of Rare Earths, Baotou 014030, China
Abstract：The content of rare earth elements in rare earth-aluminum intermediate alloy was usually 0.5%-20% (mass fraction, similarly hereinafter). The certified reference materials of rare earth-aluminum intermediate alloy as well as the determination method of rare earths with content higher than 10% was rarely reported in the literature. Lβ1 line of Sm, Lα line of La and Ce, Kα line of Y were selected as the analytical lines. The standard solutions were prepared with pure substances to solve the problem of no certified reference materials. The matrix effect was corrected by the characteristic/scattering ratio method. The fusion conditions and instrumental parameters were optimized. Thus, a determination method of rare earth elements in rare earth-aluminum intermediate alloy was established by X-ray fluorescence spectrometry (XRF) with fusion sample preparation. The results showed that the optimal sample fusion conditions were as follows: 0.2g of sample was melted with 5mL of hydrochloric acid (1+1); the mixture of lithium tetraborate and lithium metaborate was used as flux; the dilution ratio was 1∶30; 4mL of ammonium bromide solution was used as release agent; the sample fusion temperature was 1050℃ and fusion time was 15min. The contents of rare earth elements in five types of rare earth-aluminum intermediate alloys (lanthanum-aluminum, cerium-aluminum, lanthanum-cerium-aluminum, samarium-aluminum and yttrium-aluminum) were determined according to the experimental method. The results were consistent with the results obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES), and the relative standard deviations (RSDs) of determination results were all less than 2%. The proposed method was applicable for the determination of lanthanum, cerium, samarium and yttrium (0.5%-20%) in five types of rare earth-aluminum intermediate alloys including lanthanum-aluminum, cerium-aluminum, lanthanum-cerium-aluminum, samarium-aluminum and yttrium-aluminum.
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