Plutonium determination is an essential aspect of safeguards operations of spent nuclear fuel reprocessing facilities. High resolution X-ray (hiRX) is a new technique based on monochromatic wavelength dispersive X-ray fluorescence (MWDXRF) which was developed for quantification of plutonium in spent fuel. hiRX is a highly sensitive and selective technique due to the use of doubly curved crystal optics (DCCs), which provide monochromatic excitation and detection, resulting in high signal-to-noise ratio for the analyte. A benchtop prototype hiRX instrument has been tested with actual spent fuel samples from a reprocessing environment. A custom-designed ultralow volume sample cell, which contains 5 µL of liquid sample when filled with a pipette, was used in the field testing. Calibration was performed using aqueous standards containing plutonium and uranium, since uranium is the primary matrix element of spent fuel and may be present in amounts greater than 100:1 (U:Pu, g/L). Analytical results including accuracy, precision, and limit of detection (LOD) will be presented and compared with laboratory validation results. Linear response (&gt;0.99) over nearly 4 orders of magnitude and LOD of 0.7 ng/µL were demonstrated in the laboratory using strontium as a model element for plutonium. hiRX offers an alternative, nondestructive assay which can provide rapid, direct plutonium quantification in a simple to operate platform. These specific results demonstrate the potential of hiRX for more general analytical applications for sensitive and selective elemental analyses. LA-UR-14-26389<br/>

Determination of Pu in spent nuclear fuel: Results from field testing of high resolution X-ray (hiRX)

249th National Meeting (2015)

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