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All sources NASA NTRS DOE OSTI

DOE OSTI2016

Sludge batch 9 (SB9) acceptance evaluation. Radionuclide concentrations in tank 51 SB9 qualification sample prepared at SRNL

Presented in this report are radionuclide concentrations required as part of the program of qualifying Sludge Batch 9 (SB9) for processing in the Defense Waste Processing Facility (DWPF). The SB9 material is currently in Tank 51 and has been washed and prepared for transfer to Tank 40. The acceptance evaluation needs to be completed prior to the transfer of the material in Tank 51 to Tank 40. The sludge slurry in Tank 40 has already been qualified for DWPF processing and is currently being processed as Sludge Batch 8 (SB8). The radionuclide concentrations were measured or estimated in the Tank 51 SB9 Washed Qualification Sample prepared at Savannah River National Laboratory (SRNL). This sample was prepared from a three liter sample of Tank 51 sludge slurry (HTF-51-15-81) taken on July 23, 2015. The sample was delivered to SRNL where it was initially characterized in the Shielded Cells. Under the direction of Savannah River Remediation (SRR) it was then adjusted per the Tank Farm washing strategy as of October 20, 2015. This final slurry now has a composition expected to be similar to that of the slurry in Tank 51 after final preparations have been made for transfer of that slurry to Tank 40.

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DOE OSTI2015

Technologies for pre-screening IAEA swipe samples

During the course of International Atomic Energy Agency (IAEA) inspections, many samples are taken for the purpose of verifying the declared facility activities and identifying any possible undeclared activities. One of these sampling techniques is the environmental swipe sample. Due to the large number of samples collected, and the amount of time that is required to analyze them, prioritizing these swipes in the field or upon receipt at the Network of Analytical Laboratories (NWAL) will allow sensitive or mission-critical analyses to be performed sooner. As a result of this study, technologies were placed into one of three categories: recommended, promising, or not recommended. Both neutron activation analysis (NAA) and X-ray fluorescence (XRF) are recommended for further study and possible field deployment. These techniques performed the best in initial trials for pre-screening and prioritizing IAEA swipes. We learned that for NAA more characterization of cold elements (such as calcium and magnesium) would need to be emphasized, and for XRF it may be appropriate to move towards a benchtop XRF versus a handheld XRF due to the increased range of elements available on benchtop equipment. Promising techniques that will require additional research and development include confocal Raman microscopy, fluorescence microscopy, and infrared (IR) microscopy. These techniques showed substantive responses to uranium compounds, but expensive instrumentation upgrades (confocal Raman) or university engagement (fluorescence microscopy) may be necessary to investigate the utility of the techniques completely. Point-and-shoot (handheld) Raman and attenuated total reflectance–infrared (ATR-IR) measurements are not recommended, as they have not shown enough promise to continue investigations.

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DOE OSTI2015

Monitoring, Modeling, and Diagnosis of Alkali-Silica Reaction in Small Concrete Samples

Assessment and management of aging concrete structures in nuclear power plants require a more systematic approach than simple reliance on existing code margins of safety. Structural health monitoring of concrete structures aims to understand the current health condition of a structure based on heterogeneous measurements to produce high-confidence actionable information regarding structural integrity that supports operational and maintenance decisions. This report describes alkali-silica reaction (ASR) degradation mechanisms and factors influencing the ASR. A fully coupled thermo-hydro-mechanical-chemical model developed by Saouma and Perotti by taking into consideration the effects of stress on the reaction kinetics and anisotropic volumetric expansion is presented in this report. This model is implemented in the GRIZZLY code based on the Multiphysics Object Oriented Simulation Environment. The implemented model in the GRIZZLY code is randomly used to initiate ASR in a 2D and 3D lattice to study the percolation aspects of concrete. The percolation aspects help determine the transport properties of the material and therefore the durability and service life of concrete. This report summarizes the effort to develop small-size concrete samples with embedded glass to mimic ASR. The concrete samples were treated in water and sodium hydroxide solution at elevated temperature to study how ingress of sodium ions and hydroxide ions at elevated temperature impacts concrete samples embedded with glass. Thermal camera was used to monitor the changes in the concrete sample and results are summarized.

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DOE OSTI2016

Analytical results from routine DSSHT and SEHT monthly samples

Strip Effluent Hold Tank (SEHT) and Decontaminated Salt Solution Hold Tank (DSSHT) samples from several of the “microbatches” of Integrated Salt Disposition Project (ISDP) Salt Batch (“Macrobatch”) 8B have been analyzed for 238 Pu, 90 Sr, 137 Cs, cations (Inductively Coupled Plasma Emission Spectroscopy - ICPES), and anions (Ion Chromatography Anions - IC-A). The analytical results from the current microbatch samples are similar to those from previous macrobatch samples. The Cs removal continues to be excellent, with decontamination factors (DF) averaging 22,100 (114% RSD). The bulk chemistry of the DSSHT and SEHT samples does not show any signs of unusual behavior, other than lacking the anticipated degree of dilution that is calculated to occur during Modular Caustic-Side Solvent Extraction Unit (MCU) processing.

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DOE OSTI2016

Data Validation Package May 2016 Groundwater Sampling at the Bluewater, New Mexico, Disposal Site, September 2016

Groundwater samples were collected from monitoring wells at the Bluewater, New Mexico, Disposal Site to monitor groundwater contaminants as specified in the 1997 Long-Term Surveillance Plan for the DOE Bluewater (UMTRCA Title II) Disposal Site Near Grants, New Mexico (LTSP). Sampling and analyses were conducted as specified in the Sampling and Analysis Plan for U.S. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated). A duplicate sample was collected from location 16(SG).

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DOE OSTI2016

Data Validation Package May 2016 Groundwater Sampling at the Sherwood, Washington, Disposal Site August 2016

The 2001 Long-Term Surveillance Plan (LTSP) for the US. Department of Energy Sherwood Project (UMI'RCA Title II) Reclamation Cell, Wellpinit, Washington, does not require groundwater compliance monitoring at the Sherwood site. However, the LTSP stipulates limited groundwater monitoring for chloride and sulfate (designated indicator parameters) and total dissolved solids (TDS) as a best management practice. Samples were collected from the background well, MW-2B, and the two downgradient wells, MW-4 and MW-10, in accordance with the LTSP. Sampling and analyses were conducted as specified in the Sampling and Analysis Plan for US. Department of Energy Office of Legacy Management Sites (LMS/PRO/S04351, continually updated). Water levels were measured in all wells prior to sampling and in four piezometers completed in the tailings dam. Time-concentration graphs included in this report indicate that the chloride, sulfate, and TDS concentrations are consistent with historical measurements. The concentrations of chloride and sulfate are well below the State of Washington water quality criteria value of 250 milligrams per liter (mg/L) for both parameters.

2016 Groundwater Sampling Sherwood, Washington↗

DOE OSTI2019

Underground Test Area Annual Sampling Report Nevada National Security Site, Nevada (Revision 1, Calendar Year 2018)

The Sampling Plans (Rev. 0 and Rev. 1) ensure routine sampling that is critical to understanding contaminant transport near and downgradient of the underground nuclear testing areas, and is designed to ensure compliance with the UGTA Activity Quality Assurance Plan and the Federal Facility Agreement and Consent Order. This report presents the analytical data for the 2018 calendar year (CY) (January 1 through December 31, 2018) to ensure that the Sampling Plans’ objectives are achieved. Appendix D presents data from samples collected in 2016 and 2017. These results were not reported in previous reports because they were not available from the specialized laboratories at the time of the publication of the reports.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2017

The Impact of Sampling Medium and Environment on Particle Morphology

Sampling on different substrates is commonly used in laboratory and field studies to investigate the morphology and mixing state of aerosol particles. Our focus was on the transformations that can occur to the collected particles during storage, handling, and analysis. Particle samples were prepared by electrostatic deposition of size-classified sodium chloride, sulfuric acid, and coated soot aerosols on different substrates. The samples were inspected by electron microscopy before and after exposure to various environments. For coated soot, the imaging results were compared against mass-mobility measurements of airborne particles that underwent similar treatments. The extent of sample alteration ranged from negligible to major, depending on the environment, substrate, and particle composition. We discussed the implications of our findings for cases where morphology and the mixing state of particles must be preserved, and cases where particle transformations are desirable.

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DOE OSTI2019

Multivariate Pointwise Information-Driven Data Sampling and Visualization

With increasing computing capabilities of modern supercomputers, the size of the data generated from the scientific simulations is growing rapidly. As a result, application scientists need effective data summarization techniques that can reduce large-scale multivariate spatiotemporal data sets while preserving the important data properties so that the reduced data can answer domain-specific queries involving multiple variables with sufficient accuracy. While analyzing complex scientific events, domain experts often analyze and visualize two or more variables together to obtain a better understanding of the characteristics of the data features. Therefore, data summarization techniques are required to analyze multi-variable relationships in detail and then perform data reduction such that the important features involving multiple variables are preserved in the reduced data. To achieve this, in this work, we propose a data sub-sampling algorithm for performing statistical data summarization that leverages pointwise information theoretic measures to quantify the statistical association of data points considering multiple variables and generates a sub-sampled data that preserves the statistical association among multi-variables. Using such reduced sampled data, we show that multivariate feature query and analysis can be done effectively. The efficacy of the proposed multivariate association driven sampling algorithm is presented by applying it on several scientific data sets.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2017

Immediate drop on demand technology (I-DOT) coupled with mass spectrometry via an open port sampling interface

Here, the immediate drop on demand technology to a mass spectrometer via the recently introduced open port sampling interface and ESI. A maximum sample analysis throughput of 5 s per sample was demonstrated. Signal reproducibility was 10% or better as demonstrated by the quantitative analysis of propranolol and its stable isotope-labeled internal standard propranolol-d7. The ability of the system to multiply charge and analyze macromolecules was demonstrated using the protein cytochrome c. In conclusion, this immediate drop on demand technology/open port sampling interface/ESI–MS combination allowed for the quantitative analysis of relatively small mass analytes and was used for the identification of macromolecules like proteins.

47 OTHER INSTRUMENTATION↗

DOE OSTI2012

Stochastic sampling method with MCNPX for nuclear data uncertainty propagation in criticality safety applications

In the domain of criticality safety, the efficient propagation of uncertainty in nuclear data to uncertainty in k{sub eff} is an important area of current research. In this paper, a method based on stochastic sampling is presented for uncertainty propagation in MCNPX calculations. To that aim, the nuclear data (i.e. cross sections) are assumed to have a multivariate normal distribution and simple random sampling is performed following this presumed probability distribution. A verification of the developed stochastic sampling procedure with MCNPX is then conducted using the {sup 239}Pu Jezebel experiment as well as the PB-2 BWR and TMI-1 PWR pin cell models from the Uncertainty Analysis in Modeling (UAM) exercises. For the Jezebel case, it is found that the developed stochastic sampling approach predicts similar k{sub eff} uncertainties compared to conventional sensitivity and uncertainty methods. For the UAM models, slightly lower uncertainties are obtained when comparing to existing preliminary results. Further details of these verification studies are discussed and directions for future work are outlined. (authors)

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DOE OSTI2013

Optimizing the implementation of the target motion sampling temperature treatment technique - How fast can it get?

This article discusses the optimization of the target motion sampling (TMS) temperature treatment method, previously implemented in the Monte Carlo reactor physics code Serpent 2. The TMS method was introduced in [1] and first practical results were presented at the PHYSOR 2012 conference [2]. The method is a stochastic method for taking the effect of thermal motion into account on-the-fly in a Monte Carlo neutron transport calculation. It is based on sampling the target velocities at collision sites and then utilizing the 0 K cross sections at target-at-rest frame for reaction sampling. The fact that the total cross section becomes a distributed quantity is handled using rejection sampling techniques. The original implementation of the TMS requires 2.0 times more CPU time in a PWR pin-cell case than a conventional Monte Carlo calculation relying on pre-broadened effective cross sections. In a HTGR case examined in this paper the overhead factor is as high as 3.6. By first changing from a multi-group to a continuous-energy implementation and then fine-tuning a parameter affecting the conservativity of the majorant cross section, it is possible to decrease the overhead factors to 1.4 and 2.3, respectively. Preliminary calculations are also made using a new and yet incomplete optimization method in which the temperature of the basis cross section is increased above 0 K. It seems that with the new approach it may be possible to decrease the factors even as low as 1.06 and 1.33, respectively, but its functionality has not yet been proven. Therefore, these performance measures should be considered preliminary. (authors)

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DOE OSTI2013

Reducing Contingency through Sampling at the Luckey FUSRAP Site - 13186

Typically, the greatest risk in developing accurate cost estimates for the remediation of hazardous, toxic, and radioactive waste sites is the uncertainty in the estimated volume of contaminated media requiring remediation. Efforts to address this risk in the remediation cost estimate can result in large cost contingencies that are often considered unacceptable when budgeting for site cleanups. Such was the case for the Luckey Formerly Utilized Sites Remedial Action Program (FUSRAP) site near Luckey, Ohio, which had significant uncertainty surrounding the estimated volume of site soils contaminated with radium, uranium, thorium, beryllium, and lead. Funding provided by the American Recovery and Reinvestment Act (ARRA) allowed the U.S. Army Corps of Engineers (USACE) to conduct additional environmental sampling and analysis at the Luckey Site between November 2009 and April 2010, with the objective to further delineate the horizontal and vertical extent of contaminated soils in order to reduce the uncertainty in the soil volume estimate. Investigative work included radiological, geophysical, and topographic field surveys, subsurface borings, and soil sampling. Results from the investigative sampling were used in conjunction with Argonne National Laboratory's Bayesian Approaches for Adaptive Spatial Sampling (BAASS) software to update the contaminated soil volume estimate for the site. This updated volume estimate was then used to update the project cost-to-complete estimate using the USACE Cost and Schedule Risk Analysis process, which develops cost contingencies based on project risks. An investment of $1.1 M of ARRA funds for additional investigative work resulted in a reduction of 135,000 in-situ cubic meters (177,000 in-situ cubic yards) in the estimated base volume estimate. This refinement of the estimated soil volume resulted in a $64.3 M reduction in the estimated project cost-to-complete, through a reduction in the uncertainty in the contaminated soil volume estimate and the associated contingency costs. (authors)

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DOE OSTI2019

On-Line Monitoring and Real-Time Characterization of Low Level Waste and Off-Gas Condensate Samples using Raman Spectroscopy - 19274

The demand for Hanford waste property analysis is expected to significantly increase as the U.S. Department of Energy River Protection Project progresses toward transferring waste to the Hanford Waste Treatment and Immobilization Plant. The analysis of waste includes chemical, radionuclide, and physical property characterizations, with the goal of achieving safe/informed transfer and processing. Waste sampling followed by offline laboratory analysis is the current baseline analytical approach. The addition of field-deployed/in situ instruments has the potential to provide improvements and benefits over offline analysis in the areas of 1) Worker Safety: by reducing the need for sampling and thereby reducing the need for worker interaction with waste during sample handling; 2) Operational Efficiency: by reducing analysis turnaround times and offsetting demand on analytical laboratories; and 3) Accuracy: continuous analysis of a flowing waste stream allows cumulative results to be produced for the batch, which is more representative than discrete samples of batch properties. This paper describes the development and application of an online monitor to provide chemical characterizations; specifically, Raman spectroscopy is utilized to identify and quantify tank components. Accurate quantification is achieved through the use of chemometric analysis, which can be configured to provide real-time analysis in field deployment settings. (authors)

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DOE OSTI2015

On‐Demand Ambient Ionization of Picoliter Samples Using Charge Pulses

Abstract Relay electrospray ionization (rESI) from a capillary containing a sample solution (or from an array of such capillaries) is triggered by charge deposition onto the capillary. Suitable sources of primary ions, besides electrosprays, are plasma ion and piezoelectric discharge plasma sources. With no requirement for physical contact, high‐throughput sample screening is enabled by rapidly addressing individual secondary (sample) capillaries. Sub‐pL sample volumes can be loaded and sprayed. Polar analytes, including neurotransmitters, phosphopeptides, oligonucleotides, illicit drugs, and pharmaceutical compounds are successfully ionized by rESI with concentration sensitivities (0.1 ppb for acetylcholine) which are similar to nanoESI but absolute sensitivities are orders of magnitude better. Nonpolar analytes (steroids, alkynes) are ionized by rESI using an open‐tube secondary capillary and injecting electrolytically generated metal cations from the primary electrospray.

Li, Anyin↗

DOE OSTI2015

On‐Demand Ambient Ionization of Picoliter Samples Using Charge Pulses

Li, Anyin↗

DOE OSTI2026

Effect of Sample Mass, Confinement, and Preheating Time on the Thermal Response of LLM‐105: Experiments and Kinetic Analysis

Various small-scale experiments were performed to provide data for developing a model to predict the thermal response of LLM-105 over a wide range of conditions. The thermal decomposition of LLM-105 was studied as a function of sample mass, confinement of volatile products, and preheating time in both isothermal and ramped heating experiments. The thermal decomposition of LLM-105 is a two-step process, as shown by the two exothermic peaks in the heat flow profiles, which were fitted to two nth-order autocatalytic reaction models with a similar activation energy of ∼289 kJ/mol. The magnitude and shape of these peaks varied with sample mass and confinement. Increasing sample mass enhanced the second exotherm with respect to the first one, while increasing the level of confinement promoted a transition from a sublimation-dominated regime towards thermal decomposition. The effect of LLM-105 particle size on the rate of weight loss was evident for open-pan experiments, where bigger particles sublimed at lower temperatures than smaller particles. Thermal response and solid residue composition of LLM-105 samples were analyzed following preheating for different durations. Longer preheating times caused a shift of the second exotherm to lower temperatures and a decrease in the reaction enthalpy, confirming that LLM-105 decay is a consecutive reaction mechanism, probably autocatalytic. In conclusion, the kinetic model derived from ramped experiments was validated against the measured LLM-105 fraction remaining and the enthalpy remaining of the solid residue as a function of preheating times and showed good agreement.

Chemistry - Chemical explosives↗

DOE OSTI2023

Depth profiling and standardization from the back side of a sample for accurate analyses: Emphasis on quantifying low‐fluence, shallow implants in diamond‐like carbon

Rationale Back‐side thinning of wafers is used to eliminate issues with transient sputtering when analyzing near‐surface element distributions. Precise and accurate calibrated implants are created by including a standard reference material during the implantation. Combining these methods allows accurate analysis of low‐fluence, shallow features even if matrix effects are a concern. Methods Implanted Na (<2.0 × 10 11 ions/cm 2 , peaking <50 nm) in diamond‐like carbon (DLC) film on silicon (solar wind returned by NASA's Genesis mission) was prepared for measurement as follows. Implanted surfaces of samples were epoxied to wafers and back‐side‐thinned using physical or chemical methods. Thinned samples were then implanted with reference ions for accurate quantification of the solar wind implant. Analyses used a CAMECA IMS 7f‐GEO SIMS in depth‐profiling mode. Results Back‐side‐implanted reference ions reduced the need to change sample mounts or stage position and could be spatially separated from the solar wind implant even when measuring monoisotopic ions. Matrix effects in DLC were mitigated and the need to find an identical piece of DLC for a reference implant was eliminated. Accuracy was only limited by the back‐side technique itself. Conclusions Combining back‐side depth profiling with back‐side‐implanted internal standards aides quantification of shallow mono‐ and polyisotopic implants. This technique helps mitigate matrix effects and keeps measurement conditions consistent. Depth profile acquisition times are longer, but if sample matrices are homogeneous, procedural changes can decrease measurement times.

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