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Title: Analytical methods for fissionable material determinations in the nuclear fuel cycle. Progress report, October 1, 1978-September 30, 1979

Abstract

Work continues on the development of dissolution techniques for difficult-to-dissolve nuclear materials, the development of methods and automated instruments for plutonium, uranium, and thorium determinations, and the preparation of plutonium materials for the Safeguards Analytical Laboratory Evaluation (SALE) program and distribution by the National Bureau of Standards (NBS) as standard reference materials (SRMs). We are measuring the loner plutonium isotope half-lives, evaluating the isotope correlation techniques and the chemistry involved in the mass-spectrometric ion-bead techniques, and analyzing the SALE uranium materials. Completed subtasks include evaluations of various Teflon materials to recommend those acceptable for the dissolution apparatus developed at LASL, investigations of laser-enhanced dissolution of refractory materials, determinations of diverse ion effects on the microgram-sensitive method for determining uranium, fabrication of the first automated controlled-potential coulometric analyzer for determining plutonium, preparation of a /sup 244/Pu material for distribution by NBS as a SRM, and determination of the half-life of /sup 239/Pu. Work has been started on a spectrophotometric method for determining microgram quantities of plutonium, a microcomplexometric titration method for determining uranium, the use of new reagents for separations of plutonium, the preparation and packaging of a new lot of high-purity plutonium metal for distribution by NBS as a plutoniummore » chemical SRM, and determination of half-lives of other plutonium isotopes.« less

Authors:
 [1]
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  1. (comp.)
Publication Date:
Research Org.:
Los Alamos Scientific Lab., NM (USA)
OSTI Identifier:
5381562
Report Number(s):
LA-8131-PR
TRN: 80-008484
DOE Contract Number:
W-7405-ENG-36
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL PROTECTION; 37 INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY; FISSIONABLE MATERIALS; QUANTITATIVE CHEMICAL ANALYSIS; PLUTONIUM; PLUTONIUM 241; HALF-LIFE; SAFEGUARDS; ACCOUNTING; THORIUM; URANIUM; CONTAINERS; DISSOLUTION; FUEL CYCLE; REFRACTORIES; SEPARATION PROCESSES; SPECTROPHOTOMETRY; TEFLON; TITRATION; ACTINIDE ISOTOPES; ACTINIDE NUCLEI; ACTINIDES; ALPHA DECAY RADIOISOTOPES; BETA DECAY RADIOISOTOPES; BETA-MINUS DECAY RADIOISOTOPES; CHEMICAL ANALYSIS; ELEMENTS; EVEN-ODD NUCLEI; FLUORINATED ALIPHATIC HYDROCARBONS; HALOGENATED ALIPHATIC HYDROCARBONS; HEAVY NUCLEI; ISOTOPES; MANAGEMENT; METALS; NUCLEI; ORGANIC COMPOUNDS; ORGANIC FLUORINE COMPOUNDS; ORGANIC HALOGEN COMPOUNDS; ORGANIC POLYMERS; PETROCHEMICALS; PETROLEUM PRODUCTS; PLASTICS; PLUTONIUM ISOTOPES; POLYETHYLENES; POLYMERS; POLYOLEFINS; POLYTETRAFLUOROETHYLENE; RADIOISOTOPES; TRANSURANIUM ELEMENTS; YEARS LIVING RADIOISOTOPES; 055001* - Nuclear Fuels- Safeguards, Inspection, & Accountability- Technical Aspects; 400100 - Analytical & Separations Chemistry

Citation Formats

Waterbury, G.R. Analytical methods for fissionable material determinations in the nuclear fuel cycle. Progress report, October 1, 1978-September 30, 1979. United States: N. p., 1980. Web. doi:10.2172/5381562.
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Waterbury, G.R. Analytical methods for fissionable material determinations in the nuclear fuel cycle. Progress report, October 1, 1978-September 30, 1979. United States. doi:10.2172/5381562.
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Waterbury, G.R. Sat . "Analytical methods for fissionable material determinations in the nuclear fuel cycle. Progress report, October 1, 1978-September 30, 1979". United States. doi:10.2172/5381562. https://www.osti.gov/servlets/purl/5381562.
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@article{osti_5381562,
title = {Analytical methods for fissionable material determinations in the nuclear fuel cycle. Progress report, October 1, 1978-September 30, 1979},
author = {Waterbury, G.R.},
abstractNote = {Work continues on the development of dissolution techniques for difficult-to-dissolve nuclear materials, the development of methods and automated instruments for plutonium, uranium, and thorium determinations, and the preparation of plutonium materials for the Safeguards Analytical Laboratory Evaluation (SALE) program and distribution by the National Bureau of Standards (NBS) as standard reference materials (SRMs). We are measuring the loner plutonium isotope half-lives, evaluating the isotope correlation techniques and the chemistry involved in the mass-spectrometric ion-bead techniques, and analyzing the SALE uranium materials. Completed subtasks include evaluations of various Teflon materials to recommend those acceptable for the dissolution apparatus developed at LASL, investigations of laser-enhanced dissolution of refractory materials, determinations of diverse ion effects on the microgram-sensitive method for determining uranium, fabrication of the first automated controlled-potential coulometric analyzer for determining plutonium, preparation of a /sup 244/Pu material for distribution by NBS as a SRM, and determination of the half-life of /sup 239/Pu. Work has been started on a spectrophotometric method for determining microgram quantities of plutonium, a microcomplexometric titration method for determining uranium, the use of new reagents for separations of plutonium, the preparation and packaging of a new lot of high-purity plutonium metal for distribution by NBS as a plutonium chemical SRM, and determination of half-lives of other plutonium isotopes.},
doi = {10.2172/5381562},
journal = {},
number = ,
volume = ,
place = {United States},
year = {Sat Mar 01 00:00:00 EST 1980},
month = {Sat Mar 01 00:00:00 EST 1980}
}
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Technical Report:
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DOI:  10.2172/5381562
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  • Work has continued on the development of dissolution techniques for difficult-to-dissolve nuclear materials, development of methods and automated instruments for plutonium and uranium determinations, preparation of plutonium-containing materials for the Safeguards Analytical Laboratory Evaluation (SALE) program, preparation of plutonium materials for distribution by the National Bureau of Standards (NBS) as standard reference materials (SRMs), measurement of longer plutonium isotope half-lives, and analysis of SALE uranium materials. New tasks include the development of methods and automated instruments for the determination of thorium and uranium, and an evaluation of the ion-exchange-bead technique for the mass spectrometric measurement of uranium and plutonium isotopemore » distributions. Completed tasks include the measurements of ion exchange distributions of over 50 elements on cation exchange resins from nitric acid media and anion exchange resins from hydrobromic and hydriodic acid media. Using a newly developed procedure, the LASL automated spectrophotometer was modified to determine microgram levels of uranium and to determine milligram levels of uranium and plutonium. Construction of an automated controlled-potential analyzer for the determination of plutonium is nearing completion. Apparatus and procedures for the separation and complexometric titration of thorium and uranium are being developed.« less

  • Development of dissolution techniques for difficult-to-dissolve nuclear materials, development of methods and automated instruments for plutonium and uranium determinations, preparation of plutonium-containing materials for the Safeguards Analytical Laboratory Evaluation (SALE) program, analysis of SALE uranium materials, preparation of certified reference material plutonium metal, measurement of longer plutonium isotope half-lives, and study of ion exchange behavior of elements in various media continued. Gas-solid reaction of carbonyl chloride with uranium-bearing materials at elevated temperature is superior to reaction with chlorine for uranium volatilization and separation. Neither reaction with a variety of nonaqueous solvents nor reaction with molten selenium oxide provides practical dissolutionmore » of refractory materials characteristic of nuclear fuel cycle materials. The LASL automated spectrophotometer has been used to determine 0.1-mg amounts without instrumental or procedural changes. A microgram-sensitive spectrophotometric method for uranium has been developed, and the automated spectrophotometer is being modified to its use. A controlled-potential coulometric method has been developed for selective determination of plutonium. An automated analyzer to use this method is being built. Uranium-plutonium mixed oxide powder, for SALE samples, has not remained stable during storage, but high-density pellets have. In a DOE interlaboratory program, the half-life of /sup 239/Pu has been measured, experiments on /sup 241/Pu half-life measurement are in progress, and /sup 240/Pu half-life measurement is planned. Ion exchange distributions for over 50 elements have been measured to determine cation exchange in nitric acid and anion exchange in both hydrobromic and hydriodic acids.« less

  • Progress continued on development of dissolution techniques for difficult-to-dissolve nuclear materials, development of methods and automated instruments for determinations of plutonium and uranium, preparation of plutonium-containing materials for the Safeguards Analytical Laboratory Evaluation (SALE) program, analysis of SALE uranium materials, and measurement of plutonium isotope half-lives. Gas-solid reactions at elevated temperatures using reactive gases such as chlorine continue to show promise for separating uranium from refractory materials. An extensive study of nonaqueous solvents for the dissolution of refractory materials is in progress. An extraction-separation procedure, highly specific for microgram amounts of uranium, has been developed, and its adaptation to themore » Los Alamos Scientific Laboratory (LASL) automated spectrophotometer is being evaluated. Development of an electrometric analysis method for plutonium is nearing completion, and design of an automated instrument using the method has been started. Batches of plutonium oxide and mixed uranium--plutonium, intended for issue as Secondary Reference and Calibration Test Materials, are being recharacterized for assay and isotopic contents. The half-life of /sup 239/Pu has been determined by isotope-dilution mass-spectrometric measurement of /sup 235/U grow-in as a function of time.« less

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    The performance of escape type breathing apparatus was evaluated for weight, comfort, ease of use, and protection factor (calculated from facepiece leakage). All of the devices tested provided a self-contained air supply of 5- to 15-min duration. Five of them have the provision to connect an air line but allow the use of the self-contained supply for safe egress. The air supply was stored in cylinders, tubing, or disposable containers. Respiratory inlet coverings were half masks, full facepieces, hoods, and mouthpieces. An estimate is given for the ease of quick donning. Recommendations for conditions of use of the equipment aremore » given. 8 refs., 10 figs., 3 tabs.« less

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    This report summarizes progress during the past year in the following areas of nuclear structure and reaction theory: Statistical spectroscopy, including: Random matrix methods, with applications to fluctuations in spectra and in strength distributions, and to problems of ergodicity; Group symmetries in spectral-distribution theory; Electromagnetic and ..beta.. transitions. Meson scattering and absorption by nuclei, including: general scattering theory with absorption, multiple scattering theory and its reactive content, statistical theory of absorption, theory of the absorption operator (..pi..NN vertex), theory of ..pi..N scattering. A list of publications is included.