Abstract
Isotope dilution mass spectrometry (IDMS) is an analytical technique capable of providing accurate and precise quantitation of trace isotope abundance and assay providing measurement uncertainties below 1 %. To achieve these low uncertainties, the IDMS method ideally utilizes chemically pure “spike” solutions that consist of a single highly enriched isotope that is well-characterized relating to the abundance of companion isotopes and concentration in solution. To address a current demand for accurate 137Cs/137Ba ratio measurements for “age” determination of radioactive 137Cs sources, Idaho National Laboratory (INL) is producing enriched 134Ba isotopes that are tobe used for IDMS spikes to accurately determine 137Ba accumulation from the decay of 137Cs. The final objective of this work it to provide a homogenous set of reference materials that the National Institute of Standards and Technology can certify as standard reference materials used for IDMS. The process that was developed at INL for the separation and isolation of Ba isotopes, chemical purification of the isotopes in solution, and the encapsulation of the materials will be described.
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Notes
The targets are not completely dissolved; attempts were made to adjust the acid type and concentration so to preferentially dissolve the Ba from the Al target using a leaching procedure. This still etched significant Al from the surface of the targets. Al foils are preferred over Cu foils for HNO3 dissolutions because they are not as easily dissolved during the Ba leaching process.
The instrument limit of quantification was 15 times the standard deviation of the blank divided by the slope of the calibrated instrument response for that specific isotope. The method limit of detection incorporated appropriate dilution factors that were run. The detection limit for each Ba isotope is approximately 3 ppt (ICP-MS). The detection limit for total Al is approximately 10 ppb (ICP-OES).
EiChrom Technical Data report: http://www.eichrom.com/eichrom/products/info/sr_resin.aspx.
There is a possible correlation between collection substrate density and ion collection efficiency. Substrates with higher density likely cause ions to back-scatter more readily, reducing the total number of ions collected.
This reference material is in its final stages of production/certification by INL, NBL and NIST.
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Acknowledgments
The authors wish to thank Beam Imaging Solutions Inc., the Oak Ridge National Laboratory stable isotope mass separator group, the National Institute of Standards and Technology, and the U.S Department of Homeland Security for their continued support for this work.
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Horkley, J.J., Carney, K.P., Gantz, E.M. et al. Production of highly-enriched 134Ba for a reference material for isotope dilution mass spectrometry measurements. J Radioanal Nucl Chem 305, 267–275 (2015). https://doi.org/10.1007/s10967-015-4047-z
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DOI: https://doi.org/10.1007/s10967-015-4047-z