An automated inline method for the separation of trace element impurities from uranium matrices using a 200 µL column packed with UTEVA resin is presented here utilizing an Elemental Scientific, Inc. prepFAST IC in combination with a Perkin Elmer Avio 500 ICP-OES. This method reduces human exposure to highly concentrated acids and uranium-rich samples by automating the chemistry and introduction to the ICP. Calibration standards were prepared using inline dilutions requiring a single stock standard. The separation of trace elements from uranium matrices requires samples to be prepared in 8 M HNO₃, which can be detrimental to the ICP, thus a post-column dilution step was employed to dilute the eluent matrix to 4 M HNO₃. The method was optimized for a sample-to-sample time of < 9 min and monitored 21 elements in total. Proof of concept experiments for 1 µg mL⁻¹ trace elements spiked into 0.1 vol%, 0.5 vol%, and 1.0 vol% uranium matrices resulted in < 5% relative difference and < 10% relative standard deviation for triplicate measurements of each uranium matrix analyzed. Inline dilutions (pre-column) of 2 vol% uranium + 20 µg mL⁻¹ trace elements resulted in accurate and precise measurements using dilution factors of 2×, 4×, 5×, and 20×. Method detection limits for the 21 elements (Al, B, Ba, Be, Cd, Ca, Co, Cu, Fe, Li, Pb, Mg, Mn, Ni, K, Sr, Na, V, Zn, Zr, and U) analyzed for ranged from 7 to 326 ng mL⁻¹ for 70 µL volume injections.

本文介绍了一种自动在线方法，该方法使用200 µL装有UTEVA树脂的色谱柱从铀基质中分离痕量元素杂质，该方法结合了Elemental Scientific，Inc. prepFAST IC和Perkin Elmer Avio 500 ICP-OES一起使用。这种方法通过自动化学过程和引入ICP来减少人类对高浓度酸和富铀样品的暴露。使用需要单一储备标准液的在线稀释液制备校准标准液。从铀基质中分离痕量元素需要在8 M HNO _3中制备样品，这可能对ICP有害，因此采用柱后稀释步骤将洗脱液基质稀释至4 M HNO ₃。该方法针对小于9分钟的样品到样品时间进行了优化，总共监测了21个元素。对于分别分析到每个铀基质的三次重复测量，分别掺入0.1％（体积），0.5％（体积）和1.0％（体积）铀基质中的1 µg mL ^-1微量元素的概念验证实验导致相对差异小于5％，相对标准偏差小于10％ 。在线稀释（柱前）2％（体积）铀+ 20 µg mL ^-1微量元素可使用2倍，4倍，5倍和20倍的稀释系数进行准确而精确的测量。21种元素（Al，B，Ba，Be，Cd，Ca，Co，Cu，Fe，Li，Pb，Mg，Mn，Ni，K，Sr，Na，V，Zn，Zr和U的方法检测限）分析了70 µL体积进样的7到326 ng mL ^-1的范围。