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At least 1,711 records · Page 95

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DOE OSTI2014

Integrated fiducial sample mount and software for correlated microscopy

A novel design sample mount with integrated fiducials and software for assisting operators in easily and efficiently locating points of interest established in previous analytical sessions is described. The sample holder and software were evaluated with experiments to demonstrate the utility and ease of finding the same points of interest in two different microscopy instruments. Also, numerical analysis of expected errors in determining the same position with errors unbiased by a human operator was performed. Based on the results, issues related to acquiring reproducibility and best practices for using the sample mount and software were identified. Overall, the sample mount methodology allows data to be efficiently and easily collected on different instruments for the same sample location.

36 MATERIALS SCIENCE↗

DOE OSTI2014

Mercury Source Zone Identification using Soil Vapor Sampling and Analysis

Development and demonstration of reliable measurement techniqes that can detect and help quantify the nature and extent of elemental mercury (Hg(0)) in the subsurface are needed to reduce certainties in the decision making process and increase the effectiveness of remedial actions. We conducted field tests at the Y-12 National Security Complex (NSC) in Oak Ridge, TN, to determine if sampling and analysis of Hg(0) vapors in the shallow subsurface (<0.3 m depth) can be used to as an indicator of the location and extent of Hg(0) releases in the subsurface. We constructed a rigid PVC pushprobe assembly, which was driven into the ground. Soil gas samples were collected through a sealed inner tube of the assembly and analyzed immediately in the field with a Lumex and/or Jerome Hg(0) analyzer. Time-series sampling showed that Hg vapor concentrations were fairly stable over time suggesting that the vapor phase Hg(0) was not being depleted and that sampling results were not dependent on the soil gas purge volume. Hg(0) vapor data collected at over 200 pushprobe locations at 3 different release sites correlated well to areas of known Hg(0) contamination. Vertical profiling of Hg(0) vapor concentrations conducted at 2 locations provided information on the vertical distribution of Hg(0) contamination in the subsurface. We concluded from our studies that soil gas sampling and analysis can be conducted rapidly and inexpensively at a large scale to help identify areas contaminated with Hg(0).

Watson, David B↗

DOE OSTI2014

Fluidics platform and method for sample preparation and analysis

Herein provided are fluidics platform and method for sample preparation and analysis. The fluidics platform is capable of analyzing DNA from blood samples using amplification assays such as polymerase-chain-reaction assays and loop-mediated-isothermal-amplification assays. The fluidics platform can also be used for other types of assays and analyzes. In some embodiments, a sample in a sealed tube can be inserted directly. The following isolation, detection, and analyzes can be performed without a user's intervention. The disclosed platform may also comprises a sample preparation system with a magnetic actuator, a heater, and an air-drying mechanism, and fluid manipulation processes for extraction, washing, elution, assay assembly, assay detection, and cleaning after reactions and between samples.

47 OTHER INSTRUMENTATION↗

DOE OSTI2014

Toward a Fieldable Atomic Mass Spectrometer for Safeguards Applications: Sample Preparation and Ionization

The International Atomic Energy Agency’s (IAEA’s) long-term research and development plan calls for the development of new methods to detect misuse at nuclear fuel cycle facilities such as reprocessing and enrichment plants. At enrichment plants, for example, the IAEA’s contemporary safeguards approaches are based on a combination of routine and random inspections that include collection of UF6 samples from in-process material and selected cylinders for subsequent analyses. These analyses include destructive analysis (DA) in a laboratory (typically by mass spectrometry [MS]) for isotopic characterization, and environmental sampling (ES) for subsequent laboratory elemental and isotopic analysis (also both typically by MS). One area of new method development includes moving this kind of isotope ratio analytical capability for DA and ES activities into the field. Some of the reasons for these developments include timeliness of results, avoidance of hazardous material shipments, and guidance for additional sample collecting. However, this capability does not already exist for several reasons, such as that most lab-based chemical and instrumental methods rely on laboratory infrastructure (highly trained staff, power, space, hazardous material handling, etc.) and require significant amounts of consumables (power, compressed gases, etc.). In addition, there are no currently available, fieldable instruments for atomic or isotope ratio analysis. To address these issues, Pacific Northwest National Laboratory (PNNL) and collaborator, Clemson University, are studying key areas that limit the fieldability of isotope ratio mass spectrometry for atomic ions: sample preparation and ionization, and reducing the physical size of a fieldable mass spectrometer. PNNL is seeking simple and robust techniques that could be effectively used by inspectors who may have no expertise in analytical MS. In this report, we present and describe the preliminary findings for three candidate techniques: matrix-assisted laser desorption/ionization (MALDI) MS, liquid sampling-atmospheric pressure glow discharge (LS-APGD), and laser ablation/ionization (LAI) MS at atmospheric pressure. Potential performance metrics for these techniques will be presented, including detectability, response, isotope ratio accuracy and precision, and ease of use.

Barinaga, Charles J.↗

DOE OSTI2015

Method for using polarization gating to measure a scattering sample

Described herein are systems, devices, and methods facilitating optical characterization of scattering samples. A polarized optical beam can be directed to pass through a sample to be tested. The optical beam exiting the sample can then be analyzed to determine its degree of polarization, from which other properties of the sample can be determined. In some cases, an apparatus can include a source of an optical beam, an input polarizer, a sample, an output polarizer, and a photodetector. In some cases, a signal from a photodetector can be processed through attenuation, variable offset, and variable gain.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2015

Device for high spatial resolution chemical analysis of a sample and method of high spatial resolution chemical analysis

A system and method for analyzing a chemical composition of a specimen are described. The system can include at least one pin; a sampling device configured to contact a liquid with a specimen on the at least one pin to form a testing solution; and a stepper mechanism configured to move the at least one pin and the sampling device relative to one another. The system can also include an analytical instrument for determining a chemical composition of the specimen from the testing solution. In particular, the systems and methods described herein enable chemical analysis of specimens, such as tissue, to be evaluated in a manner that the spatial-resolution is limited by the size of the pins used to obtain tissue samples, not the size of the sampling device used to solubilize the samples coupled to the pins.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Characterization of high level nuclear waste glass samples following extended melter idling

The Savannah River Site Defense Waste Processing Facility (DWPF) melter was recently idled with glass remaining in the melt pool and riser for approximately three months. This situation presented a unique opportunity to collect and analyze glass samples since outages of this duration are uncommon. The objective of this study was to obtain insight into the potential for crystal formation in the glass resulting from an extended idling period. The results will be used to support development of a crystal-tolerant approach for operation of the high-level waste melter at the Hanford Tank Waste Treatment and Immobilization Plant (WTP). Two glass pour stream samples were collected from DWPF when the melter was restarted after idling for three months. The samples did not contain crystallization that was detectible by X-ray diffraction. Electron microscopy identified occasional spinel and noble metal crystals of no practical significance. Occasional platinum particles were observed by microscopy as an artifact of the sample collection method. Reduction/oxidation measurements showed that the pour stream glasses were fully oxidized, which was expected after the extended idling period. Chemical analysis of the pour stream glasses revealed slight differences in the concentrations of some oxides relative to analyses of the melter feed composition prior to the idling period. While these differences may be within the analytical error of the laboratories, the trends indicate that there may have been some amount of volatility associated with some of the glass components, and that there may have been interaction of the glass with the refractory components of the melter. These changes in composition, although small, can be attributed to the idling of the melter for an extended period. The changes in glass composition resulted in a 70-100 °C increase in the predicted spinel liquidus temperature (TL) for the pour stream glass samples relative to the analysis of the melter feed prior to the outage. This indicates that the potential for spinel crystallization increased as a result of idling for an extended period. However, the predicted TL of the pour stream glasses remained 150-200 °C below the mean melt pool temperature of about 1125 °C during the idling period. Given the change in predicted TL over the three month outage, the results indicate that it is important to have a thorough understanding of spinel crystallization within the melter for WTP to operate with a volume percent crystallization constraint. This knowledge will enable process control routines to be developed that avoid bulk crystallization in the melter and allow for recovery from off-normal events. The current WTP crystal-tolerant glass program will develop an improved understanding of spinel crystallization in the WTP melter to allow for operation at maximum waste loading in glass composition systems limited by predictions of spinel crystallization.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Systems and methods for separating particles and/or substances from a sample fluid

Systems and methods for separating particles and/or toxins from a sample fluid. A method according to one embodiment comprises simultaneously passing a sample fluid and a buffer fluid through a chamber such that a fluidic interface is formed between the sample fluid and the buffer fluid as the fluids pass through the chamber, the sample fluid having particles of interest therein; applying a force to the fluids for urging the particles of interest to pass through the interface into the buffer fluid; and substantially separating the buffer fluid from the sample fluid.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2017

Quantitative Digital Autoradiography for Environmental Swipe Sample Prioritization: System design, Characterization, and Initial Measurements

Environmental sampling and sample analyses by the International Atomic Energy Agency’s (IAEA) Network of Analytical Laboratories (NWAL) is a critical technical tool used to detect facility misuse under a Comprehensive Safeguards Agreement and to verify the absence of undeclared nuclear material activities under an Additional Protocol. Currently all environmental swipe samples (ESS) are screened using gamma spectrometry and x-ray fluorescence to estimate the amount of U and/or Pu in the ESS, to guide further analysis, and to assist in the shipment of ESS to the NWAL. Quantitative Digital Autoradiography for Environmental Samples (QDARES) is being developed to complement existing techniques through the use of a portable, real-time, high-spatial-resolution camera called the Ionizing-radiation Quantum Imaging Detector (iQID). The iQID constructs a spatial map of radionuclides within a sample or surface in real-time as charged particles (betas) and photons (gamma/x-rays) are detected and localized on an event-by-event basis. Knowledge of the location and nature of radioactive hot spots on the ESS could provide information for subsequent laboratory analysis. As a nondestructive technique, QDARES does not compromise the ESS chain of custody or subsequent laboratory analysis. In this paper we will present the system design and construction, characterization measurements with calibration sources, and initial measurements of ESS.

McDonald, Benjamin S.↗

DOE OSTI2018

Initial Characterization of ATR End Box Samples

Aluminum samples taken from discarded irradiated Advanced Test Reactor fuel element end boxes (upper and lower adapter ) were characterized to determine the chemical composition and hydration state of the surface oxides. The samples were analyzed using scanning electron microscope imaging and chemical identification, x-ray diffraction to evaluate crystalline morphology, and thermogravitational analysis to determine mass loss by dehydration. The samples were acquired from the discarded fuel element components stored in the ATR fuel handling canal and transferred to the Materials and Fuels Complex for analysis. The measurements indicate that the samples have limited oxide thickness, indicating that little corrosion has occurred beyond the initial passive layer that was intentionally formed prior to irradiation. The presence of minimal aluminum oxyhydroxide suggests that there will be minimal risk to store these fuels in air with limited risk for alteration of the base passive layer. These observations will be compared against samples that will be taken of the same type of fuel that has been in dry storage for more than 10 years.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

Statistical Sampling Plan for AGR-5/6/7 Fuel Materials

Kernels, coated particles, and compacts will be manufactured to predefined specifications for irradiation in the AGR 5/6/7 experiments. Many tests will be performed for quality assurance and most of these tests correspond to criteria that have to be met with 95% confidence, based on random samples. This report describes the statistical acceptance testing methods and gives minimum sample sizes for kernels to achieve 95% confidence. Coated particles and compacts will be addressed in revisions to this report. The methods used for sample size determination are described in detail in INL/EXT 05 00349, Statistical Methods Handbook for Advanced Gas Reactor Fuel Materials (Einerson 2005). The statistical approach is to collect a representative sample, apply an acceptance test to the sample, and accept or reject the product based on this test for each criterion. The criteria or “product specifications” are contained in SPC-1352, “AGR 5/6/7 Fuel Specification,” Revision 1 and are duplicated in this plan.

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DOE OSTI2021

POST-TEST EXAMINATIONS OF A LOCA SAMPLE FROM AN IRRADIATED HIGH-BURNUP PWR M5 FUEL ROD

A LOCA integral test with high burnup PWR M5 fuel rod was conducted in the Irradiated Fuel Examination Laboratory through the complete LOCA sequence: heating the LOCA sample to 300ºC and pressurizing the internal pressure to 8.27 MPa, heating at 5ºC/s from 300 to 1200ºC, holding in steam for 90s at 1200ºC, cooling at 3ºC/s to 800ºC, followed by water quench and rapid cooling to 100ºC. After LOCA testing, examinations, such as the fuel fragmentation analysis, burst and ballooning characterization, axial strain measurement, and microstructural examinations were performed. Metallographic examinations of an as-irradiated high burnup sample adjacent to the LOCA test sample revealed a bonding layer between the fuel and cladding. The posttest LOCA examinations indicates the corrosion layer formed during normal operations in the commercial reactor might provide a protection against the steam oxidation at high temperatures for test times performed in this work. The microstructure of the as-irradiated fuel is compared to the microstructure of the post-LOCA test fuel. Posttest LOCA examination on unirradiated post-tests Zr cladding samples was conducted, which served as baseline data for in cell testing with irradiated samples. The results obtained with irradiated PWR high burnup M5 fuel rad were compared to the LOCA test data obtained with irradiated BWR high burnup Zircaloy-2 fuel rod at Argonne national Laboratory.

Yan, Yong↗

DOE OSTI2022

Flow cell sample generator

A sample generator system includes a fluid source and a flow cell. The sample generator system includes a sampling system in communication with the flow cell to eject a fluid sample through an orifice in the flow cell. The sample generator system includes a gas pressure at the orifice in the flow cell greater than or equal to a fluid pressure at the orifice in the flow cell.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

Fast image acquisition system and method using pulsed light illumination and sample scanning to capture optical micrographs with sub-micron features

An optical inspection system for detecting sub-micron features on a sample component. The system may have a controller, a camera responsive to the controller for capturing images, an objective lens able to capture submicron scale features on the sample component, and a pulsed light source. The pulsed light source may be used to generate light pulses. The camera may be controlled to acquire images, using the objective lens, only while the pulsed light source is providing light pulses illuminating a portion of the sample component. Relative movement between the sample component and the objective lens is provided to enable at least one of a desired subportion or an entirety of the sample component to be scanned with the camera.

Yoo, Jae Hyuck↗

DOE OSTI2023

Characterizing Reactor Operations from Realistic Simulated Environmental Samples: Combining High-Performance Computing and Data Analytics

Environmental sampling is a common technique employed by inspectors and facility operators in nuclear safeguards, proliferation detection, and process monitoring contexts. Interpreting measurements performed on samples or collections of samples and ensuring the information extracted is accurate and precise is difficult. To date, these analyses have relied on simulated data to enable systematic studies; however, these models are inherently limited by the fidelity of the models and the implicit spatial averaging of isotopic composition or other signatures of interest. To advance this capability, we have refined the spatial discretization and expanded the range of physics in the simulation codes we use to perform reactor simulations and depletion calculations. This allows us to generate data that are more representative of real environmental samples, especially for the length scale of the isotopic composition and associated variation. Accordingly, these new data allow a more realistic assessment of traditional and new data analytic analysis methods. Here we present motivation for developing reactor simulations using high-performance computing methods and resources, impacts of these new simulations on our assessment of data analysis and interpretation methods, and initial results of developing and systematically testing data analytic methods designed to overcome the challenges expected of real-world samples. We also quantify the performance of these analyses using defensible statistical methods.

Dayman, Ken J.↗

DOE OSTI2015

Characteristic Performance Evaluation of a new SAGe Well Detector for Small and Large Sample Geometries

Environmental scientific research requires a detector that has sensitivity low enough to reveal the presence of any contaminant in the sample at a reasonable counting time. Canberra developed the germanium detector geometry called Small Anode Germanium (SAGe) Well detector, which is now available commercially. The SAGe Well detector is a new type of low capacitance germanium well detector manufactured using small anode technology capable of advancing many environmental scientific research applications. The performance of this detector has been evaluated for a range of sample sizes and geometries counted inside the well, and on the end cap of the detector. The detector has energy resolution performance similar to semi-planar detectors, and offers significant improvement over the existing coaxial and Well detectors. Energy resolution performance of 750 eV Full Width at Half Maximum (FWHM) at 122 keV γ-ray energy and resolution of 2.0 - 2.3 keV FWHM at 1332 keV γ-ray energy are guaranteed for detector volumes up to 425 cm{sup 3}. The SAGe Well detector offers an optional 28 mm well diameter with the same energy resolution as the standard 16 mm well. Such outstanding resolution performance will benefit environmental applications in revealing the detailed radionuclide content of samples, particularly at low energy, and will enhance the detection sensitivity resulting in reduced counting time. The detector is compatible with electric coolers without any sacrifice in performance and supports the Canberra Mathematical efficiency calibration method (In situ Object Calibration Software or ISOCS, and Laboratory Source-less Calibration Software or LABSOCS). In addition, the SAGe Well detector supports true coincidence summing available in the ISOCS/LABSOCS framework. The improved resolution performance greatly enhances detection sensitivity of this new detector for a range of sample sizes and geometries counted inside the well. This results in lower minimum detectable concentrations compared to Traditional Well detectors. The SAGe Well detectors are compatible with Marinelli beakers and compete very well with semi-planar and coaxial detectors for large samples in many applications. (authors)

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

Leverage Score Sampling for Parametric PDEs (Final Technical Report)

This final technical report summarizes the accomplishments of work performed under DOE Office of Science Award DE-SC0022266, which is titled “Leverage Score Sampling for Parametric PDEs”. The goal of the project was to extend methods from Randomized Numerical Linear Algebra (RandNLA) to tackle central computational challenges in model order reduction and uncertainty quantification (UQ) for parametric partial differential equations (PDEs). In particular, we sought to use importance sampling methods originally developed for RandNLA to develop sample efficient active learning algorithms for approximating high-dimensional scalar functions, e.g. by polynomials, Gaussian process models, and simple neural networks. Such methods can be immediately applied to developing surrogate models or to approximating quantity of interest (QoI) surfaces. In the context of PDEs, each sample used for learning equates to the solution of the differential equation for a particular set of parameters, so sample efficiency translates to improved computational efficiency for a variety of downstream tasks.

97 MATHEMATICS AND COMPUTING↗

DOE OSTI2017

The Impact of Below Detection Limit Samples in (NPP) Decommissioning Residual Risk Assessment - 17033

There are some technical problems with finalizing regulations and standards that address nuclear power plant (NPP) decommissioning site soil analyses for license termination. It is difficult to know how to best include detection limit observations from site soil analysis, because typical soil collection data is reported above, at, and below the detection limit. In addition, multiple detection limits are required to adequately estimate the soil radionuclide concentrations. In the literature, researchers analyzing environmental data refer to below the detection limit observations as 'left-censored data'. Left-censored data are less than the detection limit of the instrument(s) that made the measurements. Conventional approaches to managing left-censored data either ignore or simply replace the detection limits with zero, a fraction of the detection limit, or the detection limit itself. However, these approaches are statistically biased and limited in their usefulness. The Kaplan-Meier method, robust regression on order statistics method, and maximum likelihood estimation method are proposed to estimate the left-censored data more precisely. The proposed methods are applied to data from a Monazite powder manufacturing plant and the Colorado School of Mines Research Institute. Summary statistics such as the sample mean, sample standard deviation, sample percentiles are calculated from each data set and are used in risk and volume estimation calculations. Previous environmental analyses, such as the exposure assessment, recognize the uncertainty issue that is addressed in this research using the Latin hypercube sampling approach. Next, probabilistic distributions of the input parameters are developed for the uncertainty analyses. Finally, a framework methodology depicting the decision-making process in the proposed method is presented. The framework defines the critical steps, the amount of radioactivity, types of distributions, censoring percentage, sample size, and number of detection limits; it also allows the user to select the appropriate approach based on their site-specific data and analyses. The goal of this research is to develop a more precise risk assessment, estimate of the volume of soil removal, examine potential cost savings. (authors)

22 GENERAL STUDIES OF NUCLEAR REACTORS↗