Determination of lanthanum, cerium, praseodymium, neodymiumand samarium in geological sample by X-ray fluorescencespectrometry with pressed powder pellet
A Li-li1,2, HE Pan-hong1,2, ZHANG Pan-pan2
1. Henan Nuclear Industry Radioactive Nuclide Test Centre, Zhengzhou 450044, China; 2. Henan ProvinceNuclear Geology, Zhengzhou 450044, China
Abstract：The rapid and accurate determination of La, Ce, Pr, Nd and Sm in geological sample could provide the basis for prospecting rare-earth mineral resources. The particle size and grinding method of sample were optimized. The certified reference material series of rock, soil, stream sediment, rare earth and some multi-metal series with same particle size, similar matrix, certain content gradient and wide content range compared with tested sample were selected as the calibration samples. The spectral overlapping interference was corrected by comprehensive mathematical formula. Thus,a determination method of La, Ce, Pr, Nd and Sm in geological sample by X-ray fluorescence spectrometry (XRF) with pressed powder pellet was established. The results showed that the determination results were most consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) when the particle size of sample was not less than 160-mesh (0.097mm). 60-80g of sample was ground with grinder for 4min, and the sieving rate for 160-mesh sieve was 96.7%-98.5%, which could meet the requirement in geological standard (DZ/T 0130.2-2006), i.e., ＞95%. The oversize agglomerated particle could completely pass 160-mesh sieve after gently grinding. The detection limits of elements were listed as follows: La 2.93μg/g, Ce 3.86μg/g, Pr 2.84μg/g, Nd 2.97μg/g and Sm 4.18μg/g. The actual geological sample was used to prepare seven pellets according to the experimental method. The relative standard deviations (RSDs, n=7) of the determination results for La, Ce, Pr, Nd and Sm were between 0.81% and 1.4%. The contents of La, Ce, Pr, Nd and Sm in four geologltical samples were determined according to the experimental method. The results were consistent with the reference values (the average determined multiply by ICP-MS). The certified reference materials of rare earth, soil, stream sediment and rock (one sample for each certified reference material), which was not participated in the regression of calibration curve, were determined parallelly for five times according to the experimental method. The average of determination results for each rare earth was calculated. The results showed that the determination results were all within the allowance error range.
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