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DOE OSTI2012

Characterization of Tank 16 Annulus Samples

The closure of Tank 16H will require removal of material from the annulus of the tank. Samples from Tank 16H annulus were characterized and tested to provide information to evaluate various alternatives for removing the annulus waste. The analysis found all four annulus samples to be composed mainly of Si, Na, and Al and lesser amounts of other elements. The XRD data indicate quartz (SiO 2 ) and sodium aluminum nitrate silicate hydrate (Na 8 (Al 6 Si 6 O 24 )(NO 3 ) 2 .4H 2 O) as the predominant crystalline mineral phases in the samples. The XRD data also indicate the presence of crystalline sodium nitrate, sodium nitrite, gibbsite, hydrated sodium bicarbonate, and muscovite. Based on the weight of solids remaining at the end of the test, the water leaching test results indicate approximately 20-35% of the solids dissolved after three contacts with an approximately 3:1 volume of water at 45 C. The chemical analysis of the leachates and the XRD results of the remaining solids indicate sodium salts of nitrate, nitrite, sulfate, and possibly carbonate/bicarbonate make up the majority of the dissolved material. The majority of these salts were dissolved in the first water contact and simply diluted with each subsequent water contact. The water leaching removed large amounts of the uranium in two of the samples and {approx}1/3 of the {sup 99}Tc from all four samples. Most of the other radionuclides analyzed showed low solubility in the water leaching test. The preliminary data on the oxalic acid leaching test indicate the three acid contacts at 45 C dissolved from {approx}34-47% of the solids. The somewhat higher dissolution found in the oxalic acid leaching test versus the water leaching test might be offset by the tendency of the oxalic acid solutions to take on a gel-like consistency. The filtered solids left behind after three oxalic acid contacts were sticky and formed large clumps after drying. These two observations could indicate potential processing difficulties with solutions and solids from oxalic acid leaching. The gel formation might be avoided by using larger volumes of the acid. Further testing would be recommended before using oxalic acid to dissolve the Tank 16H annulus waste to ensure no processing difficulties are encountered in the full scale process.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2012

Analysis Of DWPF Sludge Batch 7a (Macrobatch 8) Pour Stream Samples

The Defense Waste Processing Facility (DWPF) began processing Sludge Batch 7a (SB7a), also referred to as Macrobatch 8 (MB8), in June 2011. SB7a is a blend of the heel of Tank 40 from Sludge Batch 6 (SB6) and the SB7a material that was transferred to Tank 40 from Tank 51. SB7a was processed using Frit 418. During processing of each sludge batch, the DWPF is required to take at least one glass sample to meet the objectives of the Glass Product Control Program (GPCP), which is governed by the DWPF Waste Compliance Plan, and to complete the necessary Production Records so that the final glass product may be disposed of at a Federal Repository. Three pour stream glass samples and two Melter Feed Tank (MFT) slurry samples were collected while processing SB7a. These additional samples were taken during SB7a to understand the impact of antifoam and the melter bubblers on glass redox chemistry. The samples were transferred to the Savannah River National Laboratory (SRNL) where they were analyzed.

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DOE OSTI2012

Data Report on Post-Irradiation Dimensional Change of AGC-1 Samples

This report summarizes the initial dimensional changes for loaded and unloaded AGC-1 samples. The dimensional change for all samples is presented as a function of dose. The data is further presented by graphite type and applied load levels to illustrate the differences between graphite forming processes and stress levels within the graphite components. While the three different loads placed on the samples have been verified [ ref: Larry Hull’s report] verification of the AGC-1 sample temperatures and dose levels are expected in the summer of 2012. Only estimated dose and temperature values for the samples are presented in this report to allow a partial analysis of the results.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2012

Wipe Sampling Collection Efficiencies and Holding Time Studies

Despite the fact that wipe sampling is commonly performed and the data produced by this technique is used to make numerous decisions, there is not an overwhelming consensus on the best method for collecting a wipe sample. It is generally agreed that, in order to produce reproducible quantitative results, consistent wetting solvents, wipe materials, sampling techniques, and sampling areas must be used. In addition, wetting solvents should be selected with consideration of the analyte of interest and wet wipes are better than dry wipes for the collection of organic chemicals. Thus, the goal of the Lawrence Livermore National Laboratory (LLNL) study was to understand factors affecting wipe sampling for specific chemical warfare agents (CWAs), including sarin (GB), soman (GD), cyclosarin (GF), distilled sulfur mustard (HD), and O-ethyl-S-(2-diisopropylaminoethyl) methylphosphonothioate (VX), and the pesticides diazinon and malathion.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2012

Characteristics of STP Pre-2004 Archived KE Basin Sludge Samples Before and After Re-Jarring in the RPL - April 2012

This report describes results of work performed in the Shielded Analytical Laboratory (SAL) at the Pacific Northwest National Laboratory’s (PNNL) Radiochemical Processing Laboratory (RPL) with archive K East (KE) Basin sludge samples obtained before the year 2004, with some of them composited and initially characterized five years ago (Delegard et al. 2011). The previously performed testing included the physical properties determinations for selected samples (settled and particle densities, water and solids concentrations), the pH, as well as identification of crystalline phases by X-ray diffractometry (XRD) for selected samples. Another objective of the previous characterization and testing campaign was to transfer some sludge composites and individual samples into new storage containers to overcome the embrittlement effect which develops in original glass containers as a result of extended exposure to high radiation fields and which increases probability of sample loss.

K Basin↗

DOE OSTI2013

BioWatch Sample Management System (SMS) Field Operator Guide

The BioWatch Sample Management System is software developed by Los Alamos National Laboratory to support the Department of Homeland Security BioWatch program. Field Operators use the software to keep track of samples and to provide information on the sample management process to other users and software programs within BioWatch. The information tracked about a sample includes the date and time the filter media is assembled in a filter holder, deployed to the field, placed in and removed from a collector, and received from the field, and identifies who performs each task. Field Operators can also use the software to prepare and print forms to document the chain-of-custody transfer of the samples. The BioWatch SMS Field Operator Guide provides easy-to-understand procedures for each task a Field Operator performs. This guide gives basic information about using the computer and other equipment, instructions about checking and editing data, and provides reference information, including appendices of error messages and solutions, words used interchangeably, and safety warnings plus a glossary and an index.

99 GENERAL AND MISCELLANEOUS↗

DOE OSTI2013

Analytical Results For MOX Colemanite Concrete Samples Received On September 4, 2013

The Mixed Oxide Fuel Fabrication Facility (MFFF) will use colemanite bearing concrete neutron absorber panels credited with attenuating neutron flux in the criticality design analyses and shielding operators from radiation. The Savannah River National Laboratory (SRNL) is tasked with measuring the total density, partial hydrogen density, and partial boron density of the colemanite concrete. SRNL received three samples of colemanite concrete for analysis on September 4, 2013. The average total density of each of the samples measured by the ASTM method C 642, the average partial hydrogen density was measured using method ASTM E 1131, and the average partial boron density of each sample was measured according to ASTM C 1301. The lower limits and measured values for the total density, hydrogen partial density, and boron partial density are presented. For all the samples tested, the total density and the boron partial density met or exceeded the specified limit. None of the samples met the lower limit for hydrogen partial density.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2013

Results for the Independent Sampling and Analysis of Used Oil Drums at the Impact Services Facility in Oak Ridge, Tennessee

The U.S. Department of Energy (DOE) requested that Oak Ridge Associated Universities (ORAU), via the Oak Ridge Institute for Science and Education (ORISE) contract, perform independent sampling and analysis of used oils contained within eight 55 gallon drums stored at the former IMPACT Services facility, located at the East Tennessee Technology Park in Oak Ridge, Tennessee. These drums were originally delivered by LATA Sharp Remediation Services (LSRS) to IMPACT Services on January 11, 2011 as part of the Bldg. K-33 demolition project, and the drums plus contents should have been processed as non-hazardous non-radiological waste by IMPACT Services. LSRS received a certificate of destruction on August 29, 2012 (LSRS 2012a). However, IMPACT Services declared bankruptcy and abandoned the site later in 2012, and eight of the original eleven K-33 drums are currently stored at the facility. The content of these drums is the subject of this investigation. The original drum contents were sampled by LSRS in 2010 and analyzed for gross alpha, gross beta, and polychlorinated biphenyls (PCBs), using both compositing and grab sampling techniques. The objective of this 2013 sample and analysis effort was to duplicate, to the extent possible, the 2010 sampling and analysis event to support final disposition decisions. Part of that decision process includes either verifying or refuting the assertion that oils that are currently stored in drums at the IMPACT Services facility originated from Bldg. K-33 equipment.

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DOE OSTI2013

Analytical Results For MOX Colemanite Concrete Samples Received On November, 2013

The Mixed Oxide Fuel Fabrication Facility (MFFF) will use colemanite bearing concrete neutron absorber panels credited with attenuating neutron flux in the criticality design analyses and shielding operators from radiation. The Savannah River National Laboratory (SRNL) is tasked with measuring the total density, partial hydrogen density, and partial boron density of the colemanite concrete. SRNL received two samples of colemanite concrete for analysis on November 21, 2013. The average total density of each of the samples measured by the ASTM method C 642, the average partial hydrogen density was measured using method ASTM E 1131, and the average partial boron density of each sample was measured according to ASTM C 1301. For all the samples tested, the total density and the boron partial density met or exceeded the specified limit. None of the samples met the lower limit for hydrogen partial density.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2012

January 2012 Groundwater Sampling at the Gnome-Coach, New Mexico, Site (Data Validation Package)

Annual sampling was conducted January 18, 2012, to monitor groundwater for potential radionuclide contamination at the Gnome-Coach site in New Mexico. The sampling was performed as specified in the Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites (LMS/PLN/S04351, continually updated). Well LRL-7 was not sampled per instruction from the lead. A duplicate sample was collected from well USGS-1 and water levels were measured in the monitoring wells onsite.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2013

May 2013 Groundwater and Surface Water Sampling at the Rio Blanco, Colorado, Site (Data Validation Package)

Annual sampling was conducted at the Rio Blanco, Colorado, site for the Long-Term Hydrologic Monitoring Program May 14-16, 2013, to monitor groundwater and surface water for potential radionuclide contamination. Sampling and analyses were conducted as specified in Sampling and Analysis Plan for the U.S. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated). A duplicate sample was collected from location CER #1 Black Sulphur. Samples were analyzed for gamma-emitting radionuclides by high-resolution gamma spectrometry and for tritium using the conventional and enrichment methods.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2012

May 2012 Groundwater and Surface Water Sampling at the Rio Blanco, Colorado, Site (Data Validation Package)

Annual sampling was conducted at the Rio Blanco, Colorado, site for the Long-Term Hydrologic Monitoring Program May 9-10, 2012, to monitor groundwater and surface water for potential radionuclide contamination. Sampling and analyses were conducted as specified in Sampling and Analysis Plan for the U.S. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated). A duplicate sample was collected from location Johnson Artesian WL. Samples were analyzed for gamma-emitting radionuclides by high-resolution gamma spectrometry and for tritium using the conventional and enrichment methods. Results of this monitoring at the Rio Blanco site demonstrate that groundwater and surface water outside the site boundaries have not been affected by project-related contaminants.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2014

Analysis of a Uranium Oxide Sample Interdicted in Slovakia (FSC 12-3-1)

We provide a concise summary of analyses of a natural uranium sample seized in Slovakia in November 2007. Results are presented for compound identification, water content, U assay, trace element abundances, trace organic compounds, isotope compositions for U, Pb, Sr and O, and age determination using the 234 U – 230 Th and 235 U – 231 Pa chronometers. The sample is a mixture of two common uranium compounds - schoepite and uraninite. The uranium isotope composition is indistinguishable from natural; 236 U was not detected. The O, Sr and Pb isotope compositions and trace element abundances are unremarkable. The 234 U – 230 Th chronometer gives an age of 15.5 years relative to the date of analysis, indicating the sample was produced in January 1997. A comparison of the data for this sample with data in the Uranium Sourcing database failed to find a match, indicating the sample was not produced at a facility represented in the database.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2014

Analytical Results for MOX Colemanite Concrete Samples: Received on September 4, 2013

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2014

Analytical Results for MOX Colemanite Concrete Samples: Received on November 21, 2013

The Mixed Oxide Fuel Fabrication Facility (MFFF) will use colemanite bearing concrete neutron absorber panels credited with attenuating neutron flux in the criticality design analyses and shielding operators from radiation. The Savannah River National Laboratory (SRNL) is tasked with measuring the total density, partial hydrogen density, and partial boron density of the colemanite concrete. SRNL received two samples of colemanite concrete for analysis on November 21, 2013. The average total density of each of the samples measured by the ASTM method C 642, the average partial hydrogen density was measured using method ASTM E 1131, and the average partial boron density of each sample was measured according to ASTM C 1301. The lower limits and measured values for the total density, hydrogen partial density, and boron partial density are presented. For all the samples tested, the total density and the boron partial density met or exceeded the specified limit. None of the samples met the lower limit for hydrogen partial density.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2014

A New On-the-Fly Sampling Method for Incoherent Inelastic Thermal Neutron Scattering Data in MCNP6

At thermal energies, the scattering of neutrons in a system is complicated by the comparable velocities of the neutron and target, resulting in competing upscattering and downscattering events. The neutron wavelength is also similar in size to the target's interatomic spacing making the scattering process a quantum mechanical problem. Because of the complicated nature of scattering at low energies, the thermal data files in ACE format used in continuous-energy Monte Carlo codes are quite large { on the order of megabytes for a single temperature and material. In this paper, a new storage and sampling method is introduced that is orders of magnitude less in size and is used to sample scattering parameters at any temperature on-the-fly. In addition to the reduction in storage, the need to pre-generate thermal scattering data tables at fine temperatures has been eliminated. This is advantageous for multiphysics simulations which may involve temperatures not known in advance. A new module was written for MCNP6 that bypasses the current S(α,β) table lookup in favor of the new format. The new on-the-fly sampling method was tested for graphite for two benchmark problems at ten temperatures: 1) an eigenvalue test with a fuel compact of uranium oxycarbide fuel homogenized into a graphite matrix, 2) a surface current test with a \broomstick" problem with a monoenergetic point source. The largest eigenvalue difference was 152pcm for T= 1200K. For the temperatures and incident energies chosen for the broomstick problem, the secondary neutron spectrum showed good agreement with the traditional S(α,β) sampling method. These preliminary results show that sampling thermal scattering data on-the-fly is a viable option to eliminate both the storage burden of keeping thermal data at discrete temperatures and the need to know temperatures before simulation runtime.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2014

Results for the Fourth Quarter 2012 Tank 50 WAC Slurry Sample: Chemical and Radionuclide Contaminants

This report details the chemical and radionuclide contaminant results for the characterization of the 2012 Fourth Quarter sampling of Tank 50 for the Saltstone Waste Acceptance Criteria (WAC).1 Information from this characterization will be used by Waste Solidification Engineering (WSE) to support the transfer of low-level aqueous waste from Tank 50 to the Salt Feed Tank in the Saltstone Facility in Z-Area, where the waste will be immobilized. This information is also used to update the Tank 50 Waste Characterization System. The following conclusions are drawn from the analytical results provided in this report: The concentration of the reported chemical and radioactive contaminants were less than their respective WAC Limits and Targets, unless noted in this section. Norpar 13 and Isopar L have higher detection limits 5 compared with the Saltstone WAC 1 . The data provided in this report is based upon the concentrations in the sub-sample, and due to the limited solubility in aqueous solution, may not represent the concentrations of the analytes in Tank 50. Diisooctyl adipate (or diisooctyl hexanedioate) was measured at 1.30E+00 mg/L in one of two replicate measurements conducted on an at-depth sample. a The organic analysis of the at-depth sample was conducted at the request of SRR. 4 This analyte was below the detection limit in the surface sample. The low insoluble solids content increases the measurement uncertainty for insoluble species.

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DOE OSTI2015

Results of Hg Speciation Testing on DWPF Batch 735 RCT and OGCT Samples

Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team tasked the Savannah River National Laboratory (SRNL) with preparing and shipping samples for Hg speciation. The fifth shipment of samples was designated to include Defense Waste Processing Facility (DWPF) samples from Batch 735 including two Recycle Collection Tank (RCT) samples and one Off Gas Condensate Tank (OGCT) sample; both are described fully in Table 1. This work was requested by DWPF in a Technical Assistance Request (TAR).

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