Rapid determination of 237Np and Pu isotopes in water by inductively-coupled plasma mass spectrometry and alpha spectrometry

Abstract

A new method that allows rapid preconcentration and separation of plutonium and neptunium in water samples was developed for the measurement of 237 Np and Pu isotopes by inductively-coupled plasma mass spectrometry (ICP-MS) and alpha spectrometry; a hybrid approach. 238 U can interfere with 239 Pu measurement by ICP-MS as 238 UH + mass overlap and 237 Np via peak tailing. The method provide enhanced removal of uranium by separating Pu and Np initially on TEVA Resin, then moving Pu to DGA resin for additional removal of uranium. The decontamination factor for uranium from Pu is almost 100,000 and the decontamination factor for U from Np is greater than 10,000. This method uses stacked extraction chromatography cartridges and vacuum box technology to facilitate rapid separations. Preconcentration is performed using a streamlined calcium phosphate precipitation method. Purified solutions are split between ICP-MS and alpha spectrometry so that long and short-lived Pu isotopes can be measured successfully. The method allows for simultaneous extraction of 20 samples (including QC samples) in 4 to 6 hours, and can also be used for emergency response. 239

Rapid method to determine plutonium isotopes in steel samples

“…This eliminates eluting and reloading Pu to TEVA Resin multiple times. After a single elution and rapid clean-up on DGA Resin, Pu isotopes can be eluted from DGA Resin with a 5mL volume of 0.02M HCl-0.005M HF (or also with -0.01M hydroxylamine hydrochloride) and assayed by ICP-MS. [15] Apparatus Plutonium isotopic measurements were performed by alpha-particle pulse-height measurements using Passivated Implanted Planar Silicon (PIPS) detectors. The PIPS detectors have an active surface of 450 mm 2 .…”

Assessing the potential of online ICP–MS analysis to optimize Ca/matrix separation using DGA Resin for subsequent isotopic analysis

“…Therefore, DGA Resin has been applied, first and foremost, for analyte/matrix separation in the nuclear isotopic analysis. Applications include the separation of radioactive isotopes of Sr [4,5], Y [6], Po [7], Ac [8], Pu [9][10][11], Am [12], and Cm [13]. The beneficial features and characteristics of DGA Resin are also applicable for analyte/matrix separation of stable isotopes in the fields of geochemical, archaeological, environmental, and biomedical sciences.…”

Optimization of solid phase extraction chromatography for the separation of Np from U and Pu using experimental design tools in complex matrices

“…First, Np(IV) and Pu(IV) are retained in the TEVA resin and then plutonium is transferred to the DGA resin as Pu(III) by a reduction step with a mixture of ascorbic acid and ferrous nitrate. [6][7][8] Similarly, Larivière's group have introduced innovative approaches for the analysis of neptunium using a combination of TEVA and DGA resins to separate U(IV) and Np(III) 9 and a second sequential approach using two UTEVA resins and Np(VI) as a nal pre-concentration step. 10 Traditionally, radiochemical separation methodologies are developed by monitoring the inuence of one factor at a time (e.g., acidity level, type of column, redox agents, etc.)…”