Plutonium Isotopic Analysis of Nondescript Samples by Gamma-ray Spectrometry PDF Download

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A gamma-ray spectrometry system has been developed for the Savannah River Plant that when coupled with calorimetry will allow a complete nondestructive assay of various plutonium product and waste materials contained in sealed cans. The computer-based system employs two germanium detectors to obtain spectral information that is analyzed in a unique fashion to obtain plutonium isotopic ratios.

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Measurement of various U and Pu samples by gamma-ray spectrometry were performed at the Institute of Physics and Power Engineering to support physical-inventory-taking activities under the Joint US-Russian MPC and A Program. The resulting data was analyzed by several different methods which included Canberra's MGA9.63 (Pu and MOX analysis) and MGAU (U analysis), EG and G Ortec's MGA++ (Pu and MOX analysis) and U235 (U analysis), and FRAM v2.2 (U and Pu analysis) provided by Los Alamos. The results indicate that all of these codes are capable of performing the isotopic analysis adequately. However, some additional modifications may be required to permit better measurement of some of the more unusual components in the Institute of Physics and Power Engineering (IPPE) inventory to meet the demands of inventory-taking activities.

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We have initiated a feasibility study on the use of nondestructive low-energy gamma-ray spectroscopy for plutonium isotopic analysis on resin beads. Seven resin bead samples were measured, with each sample containing an average of 9 .mu.g of plutonium; the isotopic compositions of the samples varied over a wide range. The gamma-ray spectroscopy results, obtained from 4-h counting-time measurements, were compared with mass spectrometry results. The average ratios of gamma-ray spectroscopy to mass spectrometry were 1.014 +- 0.025 for 238Pu/239Pu, 0.996 +- 0.018 for 24°Pu/239Pu, and 0.980 +- 0.038 for 241Pu/239Pu. The rapid, automated, and accurate nondestructive isotopic analysis of resin beads may be very useful to process technicians and International Atomic Energy Agency inspectors. 3 refs., 1 fig., 3 tabs.

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We have designed and built a gamma-ray spectrometer system that measures the relative plutonium isotopic abundances of plutonium oxide enriched in 238Pu. The first system installed at Westinghouse Savannah River Company was tested and evaluated on plutonium oxide in stainless steel EP60/61 containers. 238Pu enrichments ranged from 20% to 85%. Results show that 200 grams of plutonium oxide in an EP60.61 container can be measured with {plus minus}0.3% precision and better than {plus minus}1.0% accuracy in the specific power using a counting time of 50 minutes. 3 refs., 2 figs.

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We discuss the general approach, computerized data analysis methods, and results of measurements used to determine the isotopic composition of plutonium by gamma-ray spectroscopy. The simple techniques are designed to be applicable to samples of arbitrary size, geometry, age, chemical, and isotopic composition. The combination of the gamma spectroscopic measurement of isotopic composition coupled with calorimetric measurement of total sample power is shown to give a totally nondestructive determination of sample plutonium mass with a precision of 0.6% for 1000-g samples of PuO2 with 12% 24°Pu content. The precision of isotopic measurements depends upon many factors, including sample size, sample geometry, and isotopic content. Typical ranges are found to be 238Pu, 1 to 10%; 239Pu, 0.1 to 0.5%; 24°Pu, 2 to 5%; 241Pu, 0.3 to 0.7%; 242Pu (determined by isotopic correlation); and 241Am, 0.2 to 10%.

Author: W. D. Ruhter
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The gamma-ray data analysis methodology originally developed for the MGA code to determine the relative detection efficiency curve may also be used to determine the relative amounts of the isotopes being measured. This analysis approach is based on the fact that the intensity of any given gamma ray from a sample is determined by the amount of the emitting isotope present in the sample, the emission probability for the gamma ray being measured, the sample self attenuation, the attenuation due to absorbers between the sample and detector, and the detector efficiency. An equation can be written that describes a measured gamma-ray peak intensity in terms of these parameters. By selecting appropriate gamma-ray peaks from the isotopes of interest, we can solve a set of equations for the values of the parameters in any particular measurement including the relative amounts of the selected isotopes. The equations representing the peak intensities are very nonlinear and require an iterative least squares method to solve. We have developed software to ensure that during the iterative process the parameters stay within their appropriate ranges and converge properly in solving the set of equations under various measurement conditions. We have utilized and reported on this approach for determining the plutonium isotopic abundances in samples enriched in Pu-238 and to determine the U-235 enrichment of uranium samples in thick-walled containers. Recently, we have used this approach to determine the plutonium isotopic abundances of plutonium samples in thick-walled containers. We will report on this most recent application, and how this general approach can be adapted quickly to any isotopic analysis problem.

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The nondestructive assay of plutonium is important as a safeguard tool in accounting for stategic nuclear material. Several nondestructive assay techniques, e.g., calorimetry and spontaneous fission assay detectors, require a knowledge of plutonium and americium isotopic ratios to convert their raw data to total grams of plutonium. This paper describes a nondestructive technique for calculating plutonium-238, plutonium-240, plutonium-241 and americium-241 relative to plutonium-239 from measured peak areas in the high resolution gamma-ray spectra of solid plutonium samples. Gamma-ray attenuation effects have been minimized by selecting sets of neighboring peaks in the spectrum whose components are due to the different isotopes. Since the detector efficiencies are approximately the same for adjacent peaks, the accuracy of the isotopic ratios are dependent on the half-lives, branching intensities and measured peak areas. The data presented describes the results obtained by analyzing gamma-ray spectra in the energy region from 120 to 700 keV. The majority of the data analyzed was obtained from plutonium material containing 6% plutonium-240. Sample weights varied from 0.25 g to approximately 1.2 kg. The methods have also been applied to plutonium samples containing up to 23% plutonium-240 with weights of 0.25 to 200g. Results obtained by gamma-ray spectroscopy are compared to chemical analyses of aliquots taken from the bulk samples.

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A nondestructive gamma-ray technique has been developed to determine plutonium isotopic ratios. The technique is based on the high-intensity, low-energy gamma rays at 43.48, 45.23, 51.63, 59.54, and 64.83 keV for 238Pu, 24°Pu, 239Pu, 241Am, and 241Pu, respectively. The results demonstrate that this technique can accurately measure plutonium samples in a timely manner and in a wide range of masses, isotopic contents, chemical forms, and ages from chemical processing.

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An automated at-line plutonium isotopic analysis system for small-product plutonium samples in the range of 10 to 1000 .mu.g has been developed. The analysis is based on low-energy gamma rays at 43.48 keV (238Pu), 45.23 keV (24°Pu), 51.63 keV (239Pu), 64.83 keV (241Pu-237U), 129.3 keV (239Pu), and 148.6 keV (241Pu). Within a 20-ks counting time, we demonstrated that for plutonium masses> 600 .mu.g the precision is

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The Lawrence Livermore National Laboratory develops sophisticated gamma-ray analysis codes for isotopic determinations of nuclear materials based on the principles of the MultiGroup Analysis (MGA). MGA methodology has been upgraded and expanded and is now comprised of a suite of codes known as MGA++. A graphical user interface has also been developed for viewing the data and the fitting procedure. The code suite provides plutonium and uranium isotopic analysis for data collected with high-purity germanium planar and/or coaxial detector systems. The most recent addition to the MGA++ code suite, MGAHI, analyzes Pu data using higher-energy gamma rays (200 keV and higher) and is particularly useful for Pu samples that are enclosed in thick-walled containers. Additionally, the code suite can perform isotopic analysis of uranium spectra collected with cadmium-zinc-telluride (CZT) detectors. We are currently developing new codes with will integrate into the MGA++ suite. These will include Pu isotopic analysis capabilities for data collected with CZT detectors, and U isotopic analysis with high-purity germanium detectors, which utilizes only higher energy gamma rays. Future development of MGA++ will include a capability for isotopic analyses on mixtures of Pu and U.