Novel sample introduction system to reduce ICP-OES sample size for plutonium metal trace impurity determination

Abstract

A new methodology for trace elemental analysis in plutonium metal samples was developed by interfacing the novel micro-FAST sample introduction system with an ICP-OES instrument. This integrated system, especially when coupled with a low flow rate nebulization technique, reduced the sample volume requirement significantly. Improvements to instrument sensitivity and measurement precision, as well as long term stability, were also achieved by this modified ICP-OES system. The sample size reduction, together with other instrument performance merits, is of great significance, especially to nuclear material analysis.

Solid-phase extraction microfluidic devices for matrix removal in trace element assay of actinide materials

“…A total sample uptake of 1 mL was achieved using a low flowrate nebulization technique and an 800-µL sample loop. Detailed operating conditions have been described previously [8].…”

“…With the advent of low-flow nebulization and loop injection techniques for plasma spectroscopy, it is now possible to perform comprehensive, high-sensitivity actinide impurity assay by ICP-OES using just 1 mL of column effluent [8]. Although microfluidic technology for actinide separation is still in its infancy [9][10][11][12], integrated microfluidic devices customized with solid-phase resins hold significant potential as lab-on-a-chip platforms for matrix removal in trace element assay and for related analyses of actinides.…”

Evaluation and Specifications for In-Line Uranium Separations Using Inductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) Detection for Trace Elemental Analysis

“…Unfortunately, for the ICP-OES measurement, the electron-rich U/Pu matrix must be removed before analysis to minimize the spectral interferences associated with the measurement. 7,15,16…”

“…5,8,9 Trace elemental analysis by ICP-MS can be performed by diluting the sample such that the matrix (e.g., U or Pu) is at low concentrations, typically 100-500 mg g -1 , to provide accurate determinations of the impurities assuming there are no elements of interest which would possess matrix-based isobaric interferences. [10][11][12][13][14] For elements that are commonly hidden by isobaric interferences such as 24 Mg ( 12 C 12 C), 39 K ( 38 Ar 1 H), 40 Ca ( 40 Ar), and 56 Fe ( 40 Ar 16 O), ICP-OES is traditionally utilized. Unfortunately, for the ICP-OES measurement, the electron-rich U/Pu matrix must be removed before analysis to minimize the spectral interferences associated with the measurement.…”

“…Unfortunately, for the ICP-OES measurement, the electron-rich U/Pu matrix must be removed before analysis to minimize the spectral interferences associated with the measurement. 7,15,16 While many platforms have been previously described for separation of the uranium matrix, Eichrom's Uranium and TEtraVAlent (UTEVA) resin seems to be the most commonly employed. The UTEVA resin utilizes ion-exchange properties to capture the uranium matrix in a highly acidic mobile phase (> 1 M HNO 3 ) while allowing trace elements to elute freely.…”