TOPO萃取色层分离-ICP-MS法测定土壤中痕量铀的同位素丰度比
Determination of Uranium Isotopes Ratios in Soil by ICP-MS and TOPO Extraction Chromatography
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摘要: 为了测定土壤中痕量铀的同位素丰度比,对TOPO萃取色层分离环境样品中U的方法进行了探讨。通过对色层柱体积、吸附酸度、洗涤酸度,以及不同洗脱剂的条件实验,确定了分离流程。获得U的全程回收率为(98.1±1 5)%,对土壤样品中基体元素的去污因子为1 4×103~1 8×105。通过对不同丰度铀同位素标样的测量,确定了ICP MS测量铀同位素的质量偏倚系数。采用了扫描和跳峰两种数据采集方式,获得235U/238U的相对标准偏差优于1%,234U/235U,236U/235U,234U/238U和236U/238U的相对标准偏差优于5%。两种方式测量实际样品的结果吻合。Abstract: An efficient separation procedure for uranium from soils by TOPO chromatographic extraction has been developed. The procedure has been optimized experimentally for the size of the column, different concentrations of nitric acid for column load, column rinse and the different types of eluant. Uranium is recovered with approximately 98.1% efficiency by the improved and optimized procedure. The decontamination factors for the soil matrix is approximately 1.4×10~3 up to 1.8×10~5.The instrumental mass bias is usually calculated from the analyses of reference materials with certified isotope abundance ratios. For both scan and jump mode the isotope discrimination correction are evaluated and the relative standard derivations(s_r) are compared. The results show good agreement for both modes. The s_r of the isotope abundance ratio~(235)U/~(238)U is better than 1% whereas those for~(234)U/~(235)U,~(236)U/~(235)U,~(234)U/~(238)U and~(236)U/~(238)U are better than 5%.