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ICP-MS is becoming a competitive technique for measurement of plutonium isotopes. Besides the abundance sensitivity (tailing of 238 U to m / z = 239 and 240), isobaric and polyatomic ions interferences (e.g., 238 U 1 H + ) are the most critical challenges for determination of low-level plutonium in high uranium samples. This work presents a new method to solve this problem using ICP-MS with two tandem quadrupole separators and a dynamic collision/reaction cell combined with chemical separation. The interference of uranium hydrides ( 238 U 1 H + and 238 U 1 H 2  + ) was effectively eliminated using CO 2 as reaction gas by converting hydrides to oxides of uranium ions (UO + /UO 2  + ) but still keeping the intensity of the Pu + signal. The tailing interference of 238 U + (abundance sensitivity) was intensively eliminated by significantly suppressing the 238 U + signal using CO 2 as reaction gas and using two tandem quadrupole mass separators in the ICP-MS/MS. With these approaches the overall interference of uranium was reduced to &lt;1 × 10 -8 , which is 3 orders of magnitude better than the conventional ICP-MS. Combined with chemical separation with a decontamination factor of 10 5 for uranium, an overall factor of 10 12 for elimination of uranium interference was achieved. The developed method was demonstrated to enable accurate determination of &lt;10 -15 g/g level plutonium isotopes in environmental samples even in a uranium debris sample with a U/Pu atomic ratio of up to 10 12 . The developed method was validated by analysis of a spiked solution and certified reference materials of soil.

analytical chemistry

Determination of Femtogram-Level Plutonium Isotopes in Environmental and Forensic Samples with High-Level Uranium Using Chemical Separation and ICP-MS/MS Measurement