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Straightforward determination of U, Th, and Hf at trace levels using ultrasonic nebulization and axial view ICP OES

机译:使用超声波雾化和轴向观察ICP OES直接测定痕量水平的U,Th和Hf

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摘要

Inductively coupled plasma optical emission spectrometry (ICP OES) is applied for direct determination of U, Th and Hf in environmental and geological samples (phosphate rock, soil, sediment, bush branches and leaves, and natural water). Several spectral lines and sample decomposition procedures were investigated with respect to spectral and non-spectral interference. For U and Hf determination, the geological sample treatment required hydrofluoric acid, whereas Th could be accurately determined in the samples decomposed by aqua regia solely. Ultrasonic nebulization (USN) and pneumatic nebulization with aerosol desolvation (PN-DES), with and without a microporous membrane, were evaluated for introducing the sample solution into the ICP. Better results were obtained by using USN; the limits of detection for U (U II 409.014 nm), Th (Th II 401.913 nm) and Hf (Hf II 264.141 nm) were 0.03, 0.01, and 0.01 mu g g(-1), respectively. Uranium, Th and Hf were precisely and accurately determined without matrix separation/analyte pre-concentration; the relative standard deviation (RSD) was typically <7% and the recovery of the analytes in the certified reference materials (phosphate rock, soil, sediment, bush, branches and leaves, and natural water) ranged from 83 to 112%. These results were linked to careful selection of spectral lines, which depended on the sample matrix and reagents used for sample decomposition.
机译:电感耦合等离子体发射光谱法(ICP OES)用于直接测定环境和地质样品(磷酸盐岩石,土壤,沉积物,灌木树枝和树叶以及天然水中)中的U,Th和Hf。针对光谱和非光谱干扰,研究了几种光谱线和样品分解程序。对于U和Hf的测定,地质样品处理需要氢氟酸,而仅由王水分解的样品中的Th可以准确测定。评估有无微孔膜的超声雾化(USN)和带气溶胶脱气的气动雾化(PN-DES),以将样品溶液引入ICP。使用USN可获得更好的结果。 U(U II 409.014 nm),Th(Th II 401.913 nm)和Hf(Hf II 264.141 nm)的检出限分别为0.03、0.01和0.01μg g(-1)。无需基质分离/分析物预富集即可准确,准确地测定铀,Th和Hf。相对标准偏差(RSD)通常小于7%,认证参考物质(磷酸盐岩石,土壤,沉积物,灌木,树枝和树叶以及天然水)中分析物的回收率在83%至112%之间。这些结果与仔细选择光谱线有关,光谱线取决于样品基质和用于样品分解的试剂。

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