Rapid and Simultaneous Determination of Pu, Pu, Pu, and Pu in Samples with High-Level Uranium Using ICP-MS/MS and Extraction Chromatography.

As the most important plutonium isotopes, Pu, Pu, Pu, and Pu are normally measured by two to three techniques, which are tedious, time-consuming, and not suitable for rapid analysis in emergency situations. Recently, ICP-MS has become a competitive technique for the rapid measurement of Pu, Pu, and Pu. However, ICP-MS is difficult to measure Pu due to the serious isobaric interference of U. This work reports a rapid analytical method to solve this problem for the simultaneous determination of Pu, Pu, Pu, and Pu using triple-quadrupole inductively coupled plasma mass spectrometry (ICP-MS/MS) combined with chemical separation. Chemical separation achieved a high decontamination factor of 2.12 × 10 for the most critical interfering element, uranium, by using two sequential TK200 columns. The interferences of UH and U were effectively eliminated by using 12 mL/min He-6 mL/min NH as the reaction gases in the octupole collision/reaction cell in ICP-MS/MS. Combined with chemical separation, the overall elimination efficiency of UH reached 3.6 × 10, which is 10 times better than the reported method. With the high U elimination efficiency of 1.12 × 10 in the ICP-MS/MS measurement, the overall removal efficiency of U reached 10, guaranteeing accurate determination of femtogram-level Pu as well as Pu, Pu, and Pu in the samples containing milligram-level U. The detection time is reduced to minutes, well fulfilling the requirement of rapid analysis. This method is validated by analyzing the standard reference material and the spiked samples.