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Title: Analysis of Selected Legacy 85Kr Samples

Abstract

Legacy samples composed of 85Kr encapsulated in solid zeolite 5A material and five small metal tubes containing a mixture of the zeolite combined with a glass matrix resulting from hot isostatic pressing have been preserved. The samples were a result of krypton R&D encapsulation efforts in the late 1970s performed at the Idaho Chemical Processing Plant. These samples were shipped to Oak Ridge National Laboratory (ORNL) in mid-FY 2014. Upon receipt the outer shipping package was opened, and the inner package, removed and placed in a radiological hood. The individual capsules were double bagged as they were removed from the inner shipping pig and placed into individual glass sample bottles for further analysis. The five capsules were then x-ray imaged. Capsules 1 and 4 appear intact and to contain an amorphous mass within the capsules. Capsule 2 clearly shows the saw marks on the capsule and a quantity of loose pellet or bead-like material remaining in the capsule. Capsule 3 shows similar bead-like material within the intact capsule. Capsule 5 had been opened at an undetermined time in the past. The end of this capsule appears to have been cut off, and there are additional saw marks on the sidemore » of the capsule. X-ray tomography allowed the capsules to be viewed along the three axes. Of most interest was determining whether there was any residual material in the closed end of Capsule 5. The images confirmed the presence of residual material within this capsule. The material appears to be compacted but still retains some of the bead-like morphology. Based on the nondestructive analysis (NDA) results, a proposed path forward was formulated to advance this effort toward the original goals of understanding the effects of extended storage on the waste form and package. Based on the initial NDA and the fact that there are at least two breached samples, it was proposed that exploratory tests be conducted with the breached specimens before opening the three intact capsules. Portions of these would be analyzed to determine the fraction of krypton/xenon remaining in the matrix and the amount of rubidium remaining in the matrix. The inner surface of the breached capsules would be examined for corrosion. The materials contained in Capsules 2 and 5 have been examined. There appears to be a relatively uniform distribution of Kr and Rb throughout the pellets examined. The chemical composition of the pellets appears to be consistent with 5A molecular sieves. The material contained within Capsule 5 showed ~1 at. % lead. The origin of the Pb is currently indeterminate. X-ray diffraction analysis shows a significant shift from the 5A structure, most likely due to the Kr encapsulation / sintering process that occurred when the samples were made. The capsule walls were also examined and showed extensive corrosion throughout. Elemental mapping of the capsule material appeared consistent with carbon steel, while the weld material appeared consistent with a stainless steel. The interior surface of the capsule appeared to have a layer of material containing Al, Si, and Ca similar to the 5A molecular sieve. Analysis for Rb within the corrosion sites was inconclusive.« less

Authors:
 [1];  [1]
  1. Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Publication Date:
Research Org.:
Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)
Sponsoring Org.:
USDOE Office of Nuclear Energy (NE)
OSTI Identifier:
1330542
Report Number(s):
ORNL/TM-2016/350
AF5805010; NEAF327; TRN: US1700445
DOE Contract Number:
AC05-00OR22725
Resource Type:
Technical Report
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; 12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE WASTES FROM NUCLEAR FACILITIES; 11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS; ZEOLITES; CAPSULES; KRYPTON 85; WASTE FORMS; RUBIDIUM; LEAD; X RADIATION; KRYPTON; IDAHO CHEMICAL PROCESSING PLANT; CORROSION; HOT PRESSING; X-RAY DIFFRACTION; XENON; MATRIX MATERIALS; PELLETS; NONDESTRUCTIVE ANALYSIS; GLASS; IMAGES; MIXTURES; SINTERING; SURFACES; TOMOGRAPHY; CHEMICAL COMPOSITION; COMPACTS; SPATIAL DISTRIBUTION; LAYERS; MORPHOLOGY; STORAGE; TUBES; WALLS; AMORPHOUS STATE; PACKAGING; TIME DEPENDENCE

Citation Formats

Jubin, Robert Thomas, and Bruffey, Stephanie H. Analysis of Selected Legacy 85Kr Samples. United States: N. p., 2016. Web. doi:10.2172/1330542.
Jubin, Robert Thomas, & Bruffey, Stephanie H. Analysis of Selected Legacy 85Kr Samples. United States. doi:10.2172/1330542.
Jubin, Robert Thomas, and Bruffey, Stephanie H. 2016. "Analysis of Selected Legacy 85Kr Samples". United States. doi:10.2172/1330542. https://www.osti.gov/servlets/purl/1330542.
@article{osti_1330542,
title = {Analysis of Selected Legacy 85Kr Samples},
author = {Jubin, Robert Thomas and Bruffey, Stephanie H.},
abstractNote = {Legacy samples composed of 85Kr encapsulated in solid zeolite 5A material and five small metal tubes containing a mixture of the zeolite combined with a glass matrix resulting from hot isostatic pressing have been preserved. The samples were a result of krypton R&D encapsulation efforts in the late 1970s performed at the Idaho Chemical Processing Plant. These samples were shipped to Oak Ridge National Laboratory (ORNL) in mid-FY 2014. Upon receipt the outer shipping package was opened, and the inner package, removed and placed in a radiological hood. The individual capsules were double bagged as they were removed from the inner shipping pig and placed into individual glass sample bottles for further analysis. The five capsules were then x-ray imaged. Capsules 1 and 4 appear intact and to contain an amorphous mass within the capsules. Capsule 2 clearly shows the saw marks on the capsule and a quantity of loose pellet or bead-like material remaining in the capsule. Capsule 3 shows similar bead-like material within the intact capsule. Capsule 5 had been opened at an undetermined time in the past. The end of this capsule appears to have been cut off, and there are additional saw marks on the side of the capsule. X-ray tomography allowed the capsules to be viewed along the three axes. Of most interest was determining whether there was any residual material in the closed end of Capsule 5. The images confirmed the presence of residual material within this capsule. The material appears to be compacted but still retains some of the bead-like morphology. Based on the nondestructive analysis (NDA) results, a proposed path forward was formulated to advance this effort toward the original goals of understanding the effects of extended storage on the waste form and package. Based on the initial NDA and the fact that there are at least two breached samples, it was proposed that exploratory tests be conducted with the breached specimens before opening the three intact capsules. Portions of these would be analyzed to determine the fraction of krypton/xenon remaining in the matrix and the amount of rubidium remaining in the matrix. The inner surface of the breached capsules would be examined for corrosion. The materials contained in Capsules 2 and 5 have been examined. There appears to be a relatively uniform distribution of Kr and Rb throughout the pellets examined. The chemical composition of the pellets appears to be consistent with 5A molecular sieves. The material contained within Capsule 5 showed ~1 at. % lead. The origin of the Pb is currently indeterminate. X-ray diffraction analysis shows a significant shift from the 5A structure, most likely due to the Kr encapsulation / sintering process that occurred when the samples were made. The capsule walls were also examined and showed extensive corrosion throughout. Elemental mapping of the capsule material appeared consistent with carbon steel, while the weld material appeared consistent with a stainless steel. The interior surface of the capsule appeared to have a layer of material containing Al, Si, and Ca similar to the 5A molecular sieve. Analysis for Rb within the corrosion sites was inconclusive.},
doi = {10.2172/1330542},
journal = {},
number = ,
volume = ,
place = {United States},
year = 2016,
month = 9
}

Technical Report:

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  • Multivariate statistical techniques have been applied to study interrelationships among 12 variables within a set of 277 coals representing whole-seam channel, column, and core samples obtained from each of the 6 coal provinces of the United States, and varying in rank from lignite through anthracite. The data are maintained in computerized data base at The Pennsylvania State University Coal Research Section. The variables selected are components of the elemental analysis (carbon, oxygen, organic sulfur, hydrogen, and nitrogen), selected components of the proximate analysis (volatile matter and moisture), calorific value, reflectance of vitrinite, and the relative proportions of the 3 maceralmore » groups (total vitrinite, inertinite, and liptinite group macerals). Faactor analyses performed on the entire data set and on subsets separated on the basis of rank, geographic location, and by cluster analysis indicated that rank is the most important factor in determining the amount of variation of each data set. The rank-dependent variables for the entire data set are carbon, reflectance, oxygen, volatile matter, calorific value, and moisture. The maceral groups account for the next greatest source of variation. Organic sulfur is independent of the first 2 factors and is the third most important source of variation. Cluster analyses indicated that the most significant partitioning produces 4 groups which are differentiated primarily on the basis of rank, maceral composition, and organic sulfur content. Factor analyses of the individual groups provide insights into the coalification processes of these more homogeneous coal associations.« less
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