Determination of fifteen rare earth elements in ocean sediment, stream sediment, rock and soil samples by wavelength dispersion-energy dispersion combined type X-ray fluorescence spectrometer
LIU Ju-qin1, LI Xiao-li2
1. Tianshui Mineral Exploration Institute Test Center, Gansu Non-ferrous Metals Geological Exploration Bureau,Tianshui 741020,China; 2. Tianjin Institute of Geology and Mineral Research, Tianjin 300171, China
Abstract：During the determination of rare earth elements by wavelength dispersion X-ray fluorescence (WDXRF) spectrometer or energy dispersion X-ray fluorescence spectrometer (EDXRF), the problem of spectral interference exists. Moreover, the sensitivity of WDXRF analysis is also low. In order to solve these problems, the sample was prepared by pressed powder pellet, and then 15 rare earth elements (including La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu and Y) in ocean sediment, stream sediment, rock and soil samples were determined by the recently developed wavelength dispersion-energy dispersion combined type X-ray fluorescence spectrometer. The measuring conditions of wavelength dispersion and energy dispersion for analysis of rare earth elements were separately studied. For the determination of Dy, Eu and Tb, the WDXRF analysis with high resolution were recommend, while EDXRF analysis with high sensitivity could be employed for the determination of other 12 rare earth elements. The calibration curves were established using 45 standard samples of ocean sediment, stream sediment, rock and soil. The matrix effect was corrected by empirical coefficient method and using scattered radiation as the internal standard. Moreover, the spectral overlapping interference of rare earth elements was deducted by multiple regression method. The rare earth elements in ocean sediment, stream sediment, rock and soil samples were determined according to the experimental method, and the detection limits were in range of 0.01-2.8μg/g, which was about one order of magnitude lower than that of WDXRF. The precision test was conducted using the standard sample of stream sediment (GBW07313). The relative standard deviations (RSD, n=5) of measured results for rare earth elements were between 0.10% and 6.1%. The accuracy was investigated using four types of samples, and the analytical results were consistent with the certified values.
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LIU Ju-qin, LI Xiao-li. Determination of fifteen rare earth elements in ocean sediment, stream sediment, rock and soil samples by wavelength dispersion-energy dispersion combined type X-ray fluorescence spectrometer. , 2018, 38(5): 7-12.
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