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DOE OSTI2021

Solving the sample size problem for resource selection functions

Abstract Sample size sufficiency is a critical consideration for estimating resource selection functions (RSFs) from GPS‐based animal telemetry. Cited thresholds for sufficiency include a number of captured animals and as many relocations per animal N as possible. These thresholds render many RSF‐based studies misleading if large sample sizes were truly insufficient, or unpublishable if small sample sizes were sufficient but failed to meet reviewer expectations. We provide the first comprehensive solution for RSF sample size by deriving closed‐form mathematical expressions for the number of animals M and the number of relocations per animal N required for model outputs to a given degree of precision. The sample sizes needed depend on just 3 biologically meaningful quantities: habitat selection strength, variation in individual selection and a novel measure of landscape complexity, which we define rigorously. The mathematical expressions are calculable for any environmental dataset at any spatial scale and are applicable to any study involving resource selection (including sessile organisms). We validate our analytical solutions using globally relevant empirical data including 5,678,623 GPS locations from 511 animals from 10 species (omnivores, carnivores and herbivores living in boreal, temperate and tropical forests, montane woodlands, swamps and Arctic tundra). Our analytic expressions show that the required M and N must decline with increasing selection strength and increasing landscape complexity, and this decline is insensitive to the definition of availability used in the analysis. Our results demonstrate that the most biologically relevant effects on the utilization distribution (i.e. those landscape conditions with the greatest absolute magnitude of resource selection) can often be estimated with much fewer than animals. We identify several critical steps in implementing these equations, including (a) a priori selection of expected model coefficients and (b) regular sampling of background (pseudoabsence) data within a given definition of availability. We discuss possible methods to identify a priori expectations for habitat selection coefficients, effects of scale on RSF estimation and caveats for rare species applications. We argue that these equations should be a mandatory component for all future RSF studies.

Street, Garrett M.↗

DOE OSTI2022

A Subspace-Inclusive Sampling Method for the Computational Design of Compositionally Graded Alloys

Abstract Compositionally graded alloys, a subclass of functionally graded materials (FGMs), utilize localized variations in composition with a single metal part to achieve higher performance than traditional single material parts. In previous work [Kirk, T., Galvan, E., Malak, R., and Arroyave, R., 2018, “Computational Design of Gradient Paths in Additively Manufactured Functionally Graded Materials,” J. Mech. Des., 140, p. 111410. 10.1115/1.4040816], the authors presented a computational design methodology that avoids common issues which limit a gradient alloy’s feasibility, such as deleterious phases, and optimizes for performance objectives. However, the previous methodology only samples the interior of a composition space, meaning designed gradients must include all elements in the space throughout the gradient. Because even small amounts of additional alloying elements can introduce new deleterious phases, this characteristic often neglects potentially simpler solutions to otherwise unsolvable problems and, consequently, discourages the addition of new elements to the state space. The present work improves upon the previous methodology by introducing a sampling method that includes subspaces with fewer elements in the design search. The new method samples within an artificially expanded form of the state space and projects samples outside the true region to the nearest true subspace. This method is evaluated first by observing the sample distribution in each subspace of a 3D, 4D, and 5D state space. Next, a parametric study in a synthetic 3D problem compares the performance of the new sampling scheme to the previous methodology. Lastly, the updated methodology is applied to design a gradient from stainless steel to equiatomic NiTi that has practical uses such as embedded shape memory actuation and for which the previous methodology fails to find a feasible path.

Engineering↗

DOE OSTI2016

Single-view phase retrieval of an extended sample by exploiting edge detection and sparsity

We propose a new approach to robustly retrieve the exit wave of an extended sample from its coherent diffraction pattern by exploiting sparsity of the sample's edges. This approach enables imaging of an extended sample with a single view, without ptychography. We introduce nonlinear optimization methods that promote sparsity, and we derive update rules to robustly recover the sample's exit wave. We test these methods on simulated samples by varying the sparsity of the edge-detected representation of the exit wave. Finally, our tests illustrate the strengths and limitations of the proposed method in imaging extended samples.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2023

Alkaline-SDS cell lysis of microbes with acetone protein precipitation for proteomic sample preparation in 96-well plate format

Plate-based proteomic sample preparation offers a solution to the large sample throughput demands in the biotechnology field where hundreds or thousands of engineered microbes are constructed for testing is routine. Meanwhile, sample preparation methods that work efficiently on broader microbial groups are desirable for new applications of proteomics in other fields, such as microbial communities. Here, we detail a step-by-step protocol that consists of cell lysis in an alkaline chemical buffer (NaOH/SDS) followed by protein precipitation with high-ionic strength acetone in 96-well format. The protocol works for a broad range of microbes ( e . g ., Gram-negative bacteria, Gram-positive bacteria, non-filamentous fungi) and the resulting proteins are ready for tryptic digestion for bottom-up quantitative proteomic analysis without the need for desalting column cleanup. The yield of protein using this protocol increases linearly with respect to the amount of starting biomass from 0.5–2.0 OD*mL of cells. By using a bench-top automated liquid dispenser, a cost-effective and environmentally-friendly option to eliminating pipette tips and reducing reagent waste, the protocol takes approximately 30 minutes to extract protein from 96 samples. Tests on mock mixtures showed expected results that the biomass composition structure is in close agreement with the experimental design. Lastly, we applied the protocol for the composition analysis of a synthetic community of environmental isolates grown on two different media. This protocol has been developed to facilitate rapid, low-variance sample preparation of hundreds of samples and allow flexibility for future protocol development.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2014

Raw neutron scattering data for strain measurement of hydraulically loaded granite and marble samples in triaxial stress state

This entry contains raw data files from experiments performed on the Vulcan beamline at the Spallation Neutron Source at Oak Ridge National Laboratory using a pressure cell. Cylindrical granite and marble samples were subjected to confining pressures of either 0 psi or approximately 2500 psi and internal pressures of either 0 psi, 1500 psi or 2500 psi through a blind axial hole at the center of one end of the sample. The sample diameters were 1.5" and the sample lengths were 6". The blind hole was 0.25" in diameter and 3" deep. One set of experiments measured strains at points located circumferentially around the center of the sample with identical radii to determine if there was strain variability (this would not be expected for a homogeneous material based on the symmetry of loading). Another set of experiments measured load variation across the radius of the sample at a fixed axial and circumferential location. Raw neutron diffraction intensity files and experimental parameter descriptions are included.

15 GEOTHERMAL ENERGY↗

DOE OSTI2021

G-LiHT Campaign Leaf Sample details & photos, March 2017: Puerto Rico

This data package includes details of leaves sampled for leaf spectra and chemistry from 5 sites in Puerto Rico, in March of 2017. Sunlit canopy and shaded leaves of 66 species were collected. Data for each sample includes species, leaf age, type of analysis (spectroscopy, gas exchange, chemistry), sample number and sample photographs. The data package includes a spreadsheet with sample information and a zip file of photographs (1.6 GB). This data was collected as part of the 2017 BNL–G-LiHT leaf spectra campaign. See related datasets for leaf spectral reflectance and transmittance, leaf mass area (LMA), and leaf chemistry. Note that leaf sample details are also included in related datasets.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2014

Analytical Results for MOX Colemanite Concrete Samples Received on January 15, 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 twelve samples of colemanite concrete for analysis on January 15, 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 hydrogen partial density met or exceeded the specified limit. All of the samples met or exceeded the boron partial density lower bound with the exception of samples G3-M11-2000-H, G3-M11-3000-M, and G5-M1-3000-H which are below the limit of 1.65E-01 g/cm 3 .

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2014

Assessment of the LV-S2 & LV-S3 Stack Sampling Probe Locations for Compliance with ANSI/HPS N13.1-1999

This document reports on a series of tests conducted to assess the proposed air sampling locations for the Hanford Tank Waste Treatment and Immobilization Plant (WTP) Group 1-2A exhaust stacks with respect to the applicable criteria regarding the placement of an air sampling probe. The LV-C2, LV-S2, and LV-S3 exhaust stacks were tested together as a group (Test Group 1-2A). This report only covers the results of LV-S2 and LV-S3; LV-C2 will be reported on separately. Federal regulations1 require that a sampling probe be located in the exhaust stack according to the criteria established by the American National Standards Institute/Health Physics Society (ANSI/HPS) N13.1-1999, Sampling and Monitoring Releases of Airborne Radioactive Substances from the Stack and Ducts of Nuclear Facilities. 2 These criteria address the capability of the sampling probe to extract a sample that represents the effluent stream.

Glissmeyer, John A.↗

DOE OSTI2015

Results of Hg Speciation Testing on 2Q15 Tank 50 and Tank 21 TCLP Extraction Fluid Samples and Tank 49 Material

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences, Inc. in Seattle, WA on behalf of the Savannah River Remediation (SRR) Mercury Task Team. The sixth shipment of samples was designated to include SRNL Toxicity Characteristic Leaching Procedure (TCLP) extraction fluids from the 2Q15 Tank 50 and Tank 21 saltstone waste forms as well as Tank 49 material (HTF-49-15-45) collected on May 7, 2015. The TCLP extraction fluid samples were collected from duplicate extractions of two crushed saltstone fractions, one designated as “large” and one designated as “normal”. Both fractions of 2Q15 Tank 50 and Tank 21 saltstones (eight samples) were collected with the minimum possible free headspace and refrigerated prior to final dilution. The Tank 49 sample was left in its stainless steel dip bottle until it was opened and an aliquot diluted 1:100 with Eurofins deionized water on May 21, 2015. Following initial dilution in the Shielded Cells, the diluted Tank 49 sample was immediately moved to refrigeration and kept in the dark until prepared for shipment to Eurofins.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Analysis Of Condensate Samples In Support Of The Antifoam Degradation Study

The degradation of Antifoam 747 to form flammable decomposition products has resulted in declaration of a Potential Inadequacy in the Safety Analysis (PISA) for the Defense Waste Processing Facility (DWPF). Savannah River National Laboratory (SRNL) testing with simulants showed that hexamethyldisiloxane (HMDSO), trimethylsilanol (TMS), and 1-propanal are formed in the offgas from the decomposition of the antifoam. A total of ten DWPF condensate samples from Batch 735 and 736 were analyzed by SRNL for three degradation products and additional analytes. All of the samples were analyzed to determine the concentrations of HMDSO, TMS, and propanal. The results of the organic analysis found concentrations for propanal and HMDSO near or below the detection limits for the analysis. The TMS concentrations ranged from below detection to 11 mg/L. The samples from Batch 736 were also analyzed for formate and oxalate anions, total organic carbon, and aluminum, iron, manganese, and silicon. Most of the samples contained low levels of formate and therefore low levels of organic carbon. These two values for each sample show reasonable agreement in most cases. Low levels of all the metals (Al, Fe, Mn, and Si) were present in most of the samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

ANALYSIS OF CONDENSATE SAMPLES IN SUPPORT OF THE ANTIFOAM DEGRADATION STUDY

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2016

Radiological results for samples collected on paired glass- and cellulose-fiber filters at the Sandia complex, Tonopah Test Range, Nevada

Airborne particulates are collected at U.S. Department of Energy sites that exhibit radiological contamination on the soil surface to help assess the potential for wind to transport radionuclides from the contamination sites. Collecting these samples was originally accomplished by drawing air through a cellulose-fiber filter. These filters were replaced with glass-fiber filters in March 2011. Airborne particulates were collected side by side on the two filter materials between May 2013 and May 2014. Comparisons of the sample mass and the radioactivity determinations for the side-by-side samples were undertaken to determine if the change in the filter medium produced significant results. The differences in the results obtained using the two filter types were assessed visually by evaluating the time series and correlation plots and statistically by conducting a nonparametric matched-pair sign test. Generally, the glass-fiber filters collect larger samples of particulates and produce higher radioactivity values for the gross alpha, gross beta, and gamma spectroscopy analyses. However, the correlation between the radioanalytical results for the glass-fiber filters and the cellulose-fiber filters was not strong enough to generate a linear regression function to estimate the glass-fiber filter sample results from the cellulose-fiber filter sample results.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2015

2015 Long-Term Hydrologic Monitoring Program Sampling and Analysis Results at Rio Blanco, Colorado

The U.S. Department of Energy (DOE) Office of Legacy Management conducted annual sampling at the Rio Blanco, Colorado, Site for the Long-Term Hydrologic Monitoring Program (LTHMP) on May 20–21, 2015. This report documents the analytical results of the Rio Blanco annual monitoring event, the trip report, and the data validation package. The groundwater and surface water monitoring samples were shipped to the GEL Group Inc. laboratories for conventional analysis of tritium and analysis of gamma-emitting radionuclides by high-resolution gamma spectrometry. A subset of water samples collected from wells near the Rio Blanco site was also sent to GEL Group Inc. for enriched tritium analysis. All requested analyses were successfully completed. Samples were collected from a total of four onsite wells, including two that are privately owned. Samples were also collected from two additional private wells at nearby locations and from nine surface water locations. Samples were analyzed for gamma-emitting radionuclides by high-resolution gamma spectrometry, and they were analyzed for tritium using the conventional method with a detection limit on the order of 400 picocuries per liter (pCi/L). Four locations (one well and three surface locations) were analyzed using the enriched tritium method, which has a detection limit on the order of 3 pCi/L. The enriched locations included the well at the Brennan Windmill and surface locations at CER-1, CER-4, and Fawn Creek 500 feet upstream.

54 ENVIRONMENTAL SCIENCES↗

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 Actinide Removal Process (ARP) and the Modular Caustic-Side Solvent Extraction Unit (MCU) continue to show more than adequate Pu and Sr removal for times when monosodium titanate (MST) is used. Even with no MST strike being performed there exists some small Pu and Sr removal, likely from filtration of fines containing these elements. The Cs removal continues to be excellent, with decontamination factors (DF) averaging 16,400. The bulk chemistry of the DSSHT and SEHT samples do not show any signs of unusual behavior. SRNL recommends that a sample of the strip feed be analyzed for cation and anion content if a further decline in boron concentration is noted in future SEHT samples.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2016

Analysis of Selected Legacy 85 Kr Samples

Legacy samples composed of 85 Kr 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.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2016

Data Validation Package, December 2015, 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 HMC-951. Alluvium wells are completed in the alluvial sediments in the former channel of the Rio San Jose, which was covered by basalt lava flows known as the El Malpais, and are identified by the suffix (M). Bedrock wells are completed in the San Andres Limestone/Glorieta Sandstone hydrologic unit (San Andres aquifer) and are identified by the suffix (SG). Wells HMC-951 and OBS-3 are also completed in the San Andres aquifer. The LTSP requires monitoring for molybdenum, selenium, uranium, and polychlorinated biphenyls (PCBs); PCB monitoring occurs only during November sampling events. This event included sampling for an expanded list of analytes to characterize the site aquifers and to support a regional groundwater investigation being conducted by the New Mexico Environment Department.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2017

Sampling for Air Chemical Emissions from the Life Sciences Laboratory II

Sampling for air chemical emissions from the Life Science Laboratory II (LSL-II) ventilation stack was performed in an effort to determine potential exposure of maintenance staff to laboratory exhaust on the building roof. The concern about worker exposure was raised in December 2015 and several activities were performed to assist in estimating exposure concentrations. Data quality objectives were developed to determine the need for and scope and parameters of a sampling campaign to measure chemical emissions from research and development activities to the outside air. The activities provided data on temporal variation of air chemical concentrations and a basis for evaluating calculated emissions. Sampling for air chemical emissions was performed in the LSL-II ventilation stack over the 6-week period from July 26 to September 1, 2016. A total of 12 sampling events were carried out using 16 sample media. Resulting analysis provided concentration data on 49 analytes. All results were below occupational exposure limits and most results were below detection limits. When compared to calculated emissions, only 5 of the 49 chemicals had measured concentrations greater than predicted. This sampling effort will inform other study components to develop a more complete picture of a worker’s potential exposure from LSL-II rooftop activities. Mixing studies were conducted to inform spatial variation in concentrations at other rooftop locations and can be used in conjunction with these results to provide temporal variations in concentrations for estimating the potential exposure to workers working in and around the LSL-II stack.

54 ENVIRONMENTAL SCIENCES↗

DOE OSTI2018

Characterization of Tank 51 Sludge Slurry Samples (HTF-51-17-44/ HTF-51-17-48) in Support of Sludge Batch 10 Processing

The Savannah River National Laboratory (SRNL) was requested by Savannah River Remediation (SRR) Engineering (SRR-E) to provide sample characterization and analyses of Tank 51 sludge samples in support of Sludge Batch (SB) 10. The two Tank 51 sludge samples were sampled and delivered to SRNL in May of 2017. These two Tank 51 sludge samples were combined into one composite sample and analyzed for corrosion controls analytes, select radionuclides, chemical elements, density and weight percent total solids and aluminum hydroxides (gibbsite and boehmite) by x-ray diffraction.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗