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DOE OSTI2022

Meta-Study of Particulate Detection Losses on Radioactive Air Sample Filters

Several mathematical relationships between air sample filter mass loading and the correlated analytical self-absorption factor were developed using data from other published research in this meta-study. Gross-alpha and -beta applications are addressed for this research. As filter media becomes loaded with particulate matter, there is potential for measurement losses due to self-absorption by mass loading. Components contributing to absorption include particulate dust, radioactive particulates, and filter material. Standards indicate a correction factor should be used when the penetration of radioactive material into the collection media or self-absorption of radiation by the material collected would reduce the detection rate by more than 5%. Previously, losses due to self-absorption have been reported up to 100% over a range up to ~10 mg∙cm -2 mass loading. These absorption losses then can be used to determine a correction factor for sample results. For low mass loadings (e.g., ≤0.1 mg∙cm -2 ) corrections factors in the 0.85 - 1 range have been recommended and used, while at higher mass loadings nearer to 10 mg∙cm -2 correction factors closer to 0 (representing near 100% losses) are used. Based on data from published studies, the different methods for relating percent loss due to self-absorption to mass loading include linear, exponential, quadratic, and trinomial derived functions. Where applicable, both forced zero and non-forced zero results were evaluated. From the derived functions evaluated, the trinomial function provided the best fit. Once the sample filter mass loading is known, the trinomial function can be applied to estimate losses and the corresponding self-absorption factor. When applied to routine operating conditions for radiological facility stacks monitored at the Pacific Northwest National Laboratory for an average sample filter mass loading of 0.09 ± 0.12 (2σ) mg∙cm -2 (excluding negative values and outliers) and a range from 0 - 0.24 mg∙cm -2 , the estimated trinomial function nominal self-absorption losses are less than 5% at 0.09 mg∙cm -2 and less than 10% at 0.24 mg∙cm -2 . The trinomial function is one method that may be used to adjust the activity results of an air sample when the sample-specific mass loading is determined. The application of no correction factor when the ANSI/HPS N13.1-2021 guidance of a 5% threshold for loss is not reached with typical stack sample mass loadings may be reasonable in high-efficiency particulate air filtered systems. For simplicity, it would be conservative in assigning the self-absorption correction factor at the 5% threshold (i.e., 0.95) for general uses but in cases of heavy mass loading to calculate the factor.

air sampling↗

NASA NTRSDate not supplied

Mars Sample Return – An Overview of the Capture, Containment and Return System

The Mars Sample Return campaign aims at bringing back soil, rock and atmospheric samples from Mars to Earth to answer key questions about Mars’ biological evolution by means of four missions. The first one, Mars 2020, landed on the red planet on February 18, 2021 and has to date collected a number of samples through the Perseverance rover. The three subsequent missions will recover the sample tubes, launch them into Mars orbit and transport them back to Earth. These missions are currently in the planning and design stages of development and represent an international effort comprising NASA, ESA and many industry partners. The work presented here provides an overview of the current design and concept of operations of the NASA-provided Capture, Containment, and Return System (CCRS), which is the payload of the ESA-provided Earth Return Orbiter (ERO). ERO will rendezvous with the orbiting samples and CCRS will capture them, contain them and robotically insert them into a capsule that will return the samples to Earth, the Earth Entry System (EES). Three days before arrival on Earth, CCRS will release the EES, which will fly through space, enter Earth’s atmosphere, descend on a well-defined trajectory and safely land at the Utah Test and Training Range. The decision to implement Mars Sample Return will not be finalized until NASA’s completion of the National Environmental Policy Act process. This document is being made available for information purposes only.

Mars Sample Return↗

NASA NTRS2023

Stand Alone Electrical Equipment PRL 227a (Formerly PRL 227 LOC3) Confirmatory Sampling Report Addendum

HydroGeoLogic, Inc. (HGL) prepared this Confirmatory Sampling Report Addendum (CSRA) for the National Aeronautics and Space Administration (NASA), Kennedy Space Center (KSC), Florida. PRL 227a Location of Concern (LOC) 3 is located on 10th Street, west of the former Vertical Processing Facility (M7-1469), SWMU 077. The Load Break Switches (LBS) were installed in 1986 and are suspected to have formerly contained dielectric fluid that contained polychlorinated biphenyls (PCBs). The LBS were replaced in 1993 with new LBSs that do not contain PCBs. The LBS are located on a concrete pad surrounded by grass that is mowed and maintained. A total of 330 soil samples were collected between June 2020 and December 2022 from 88 locations at depths ranging from 0-0.5 to 19-20 ft bls. In general, soil samples collected from depths less than 5 ft were collected via hand auger and samples collected beyond 5 ft bls were collected using a direct-push technology drill rig. Soil samples collected from greater than 5 ft bls to 20 ft bls were collected to confirm PCBs were not present at depth in the aquifer matrix. Delineation samples were collected using an approximately 20 ft horizontal spacing. PCB impacted soil has been completely delineated to the State of Florida residential soil cleanup target level (SCTL) at PRL 227a horizontally and vertically. PCB concentrations have been identified above the residential and industrial SCTL as well as concentrations greater than or equal to 50 ppm requiring coordination with EPA and disposal at a facility authorized under TSCA. Based upon the CSRA sampling, an interim measure is recommended to remove PCB impacted soil above the residential SCTL. The total volume of PCB impacted soil to be removed is 591.6 cubic yards. This includes approximately 9.3 cubic yards of soil with PCB concentrations greater than or equal to 50 ppm. An interim measure work plan is included as an attachment to this report.

electrical equipment↗

NASA NTRSDate not supplied

The Venus Atmospheric Sample Return (VATMOS-SR) Mission Concept

VATMOS-SR (Venus ATMOSpheric - Sample Return) is a small space- craft mission concept that would return several gas samples from the upper atmosphere of Venus (< 110 km) to Earth for scientific analysis. This could be the first sample return mission for an extraterrestrial atmosphere and potentially the first sample return from an Earth-sized planet. The VATMOS-SR mission concept consists of a SmallSat atmospheric sampling probe (45 deg. sphere/cone geometry, <1 m diameter) that is designed to skim through the Venus upper atmosphere and ac- quire gas samples below the homopause altitude (around ~110 km altitude), where the different atmospheric gases are mixed. The velocity of the spacecraft where sampling would occur is expected to be between ~10.5 km/s and ~13.1 km/s, depending on the trajectory chosen (e.g. trajectory shown in Fig. 1).

direct simulation Monte Carlo↗

NASA NTRSDate not supplied

The Venus Atmospheric Sample Return (VATMOS-SR) Mission Concept

direct simulation Monte Carlo↗

DOE OSTI2017

Method for Hot Real-Time Sampling of Gasification Products

The Thermochemical Process Development Unit (TCPDU) at the National Renewable Energy Laboratory (NREL) is a highly instrumented half-ton/day pilot scale plant capable of demonstrating industrially relevant thermochemical technologies from lignocellulosic biomass conversion, including gasification. Gasification creates primarily Syngas (a mixture of Hydrogen and Carbon Monoxide) that can be utilized with synthesis catalysts to form transportation fuels and other valuable chemicals. Biomass derived gasification products are a very complex mixture of chemical components that typically contain Sulfur and Nitrogen species that can act as catalysis poisons for tar reforming and synthesis catalysts. Real-time hot online sampling techniques, such as Molecular Beam Mass Spectrometry (MBMS), and Gas Chromatographs with Sulfur and Nitrogen specific detectors can provide real-time analysis providing operational indicators for performance. Sampling typically requires coated sampling lines to minimize trace sulfur interactions with steel surfaces. Other materials used inline have also shown conversion of sulfur species into new components and must be minimized. Sample line Residence time within the sampling lines must also be kept to a minimum to reduce further reaction chemistries. Solids from ash and char contribute to plugging and must be filtered at temperature. Experience at NREL has shown several key factors to consider when designing and installing an analytical sampling system for biomass gasification products. They include minimizing sampling distance, effective filtering as close to source as possible, proper line sizing, proper line materials or coatings, even heating of all components, minimizing pressure drops, and additional filtering or traps after pressure drops.

09 BIOMASS FUELS↗

NASA NTRS2012

Evaluating Core Quality for a Mars Sample Return Mission

Sample return missions, including the proposed Mars Sample Return (MSR) mission, propose to collect core samples from scientifically valuable sites on Mars. These core samples would undergo extreme forces during the drilling process, and during the reentry process if the EEV (Earth Entry Vehicle) performed a hard landing on Earth. Because of the foreseen damage to the stratigraphy of the cores, it is important to evaluate each core for rock quality. However, because no core sample return mission has yet been conducted to another planetary body, it remains unclear as to how to assess the cores for rock quality. In this report, we describe the development of a metric designed to quantitatively assess the mechanical quality of any rock cores returned from Mars (or other planetary bodies). We report on the process by which we tested the metric on core samples of Mars analogue materials, and the effectiveness of the core assessment metric (CAM) in assessing rock core quality before and after the cores were subjected to shocking (g forces representative of an EEV landing).

Mars samples↗

DOE OSTI2024

Brain‐age prediction: Systematic evaluation of site effects, and sample age range and size

Abstract Structural neuroimaging data have been used to compute an estimate of the biological age of the brain (brain‐age) which has been associated with other biologically and behaviorally meaningful measures of brain development and aging. The ongoing research interest in brain‐age has highlighted the need for robust and publicly available brain‐age models pre‐trained on data from large samples of healthy individuals. To address this need we have previously released a developmental brain‐age model. Here we expand this work to develop, empirically validate, and disseminate a pre‐trained brain‐age model to cover most of the human lifespan. To achieve this, we selected the best‐performing model after systematically examining the impact of seven site harmonization strategies, age range, and sample size on brain‐age prediction in a discovery sample of brain morphometric measures from 35,683 healthy individuals (age range: 5–90 years; 53.59% female). The pre‐trained models were tested for cross‐dataset generalizability in an independent sample comprising 2101 healthy individuals (age range: 8–80 years; 55.35% female) and for longitudinal consistency in a further sample comprising 377 healthy individuals (age range: 9–25 years; 49.87% female). This empirical examination yielded the following findings: (1) the accuracy of age prediction from morphometry data was higher when no site harmonization was applied; (2) dividing the discovery sample into two age‐bins (5–40 and 40–90 years) provided a better balance between model accuracy and explained age variance than other alternatives; (3) model accuracy for brain‐age prediction plateaued at a sample size exceeding 1600 participants. These findings have been incorporated into CentileBrain ( https://centilebrain.org/#/brainAGE2 ), an open‐science, web‐based platform for individualized neuroimaging metrics.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2016

Extraction efficiency and implications for absolute quantitation of propranolol in mouse brain, liver and kidney thin tissue sections using droplet-based liquid microjunction surface sampling-HPLC ESI-MS/MS

Currently, absolute quantitation aspects of droplet-based surface sampling for thin tissue analysis using a fully automated autosampler/HPLC-ESI-MS/MS system are not fully evaluated. Knowledge of extraction efficiency and its reproducibility is required to judge the potential of the method for absolute quantitation of analytes from thin tissue sections. Methods: Adjacent thin tissue sections of propranolol dosed mouse brain (10- μm-thick), kidney (10- μm-thick) and liver (8-, 10-, 16- and 24- μm-thick) were obtained. Absolute concentration of propranolol was determined in tissue punches from serial sections using standard bulk tissue extraction protocols and subsequent HPLC separations and tandem mass spectrometric analysis. These values were used to determine propranolol extraction efficiency from the tissues with the droplet-based surface sampling approach. Results: Extraction efficiency of propranolol using 10- μm-thick brain, kidney and liver thin tissues using droplet-based surface sampling varied between ~45-63%. Extraction efficiency decreased from ~65% to ~36% with liver thickness increasing from 8 μm to 24 μm. Randomly selecting half of the samples as standards, precision and accuracy of propranolol concentrations obtained for the other half of samples as quality control metrics were determined. Resulting precision ( ±15%) and accuracy ( ±3%) values, respectively, were within acceptable limits. In conclusion, comparative quantitation of adjacent mouse thin tissue sections of different organs and of various thicknesses by droplet-based surface sampling and by bulk extraction of tissue punches showed that extraction efficiency was incomplete using the former method, and that it depended on the organ and tissue thickness. However, once extraction efficiency was determined and applied, the droplet-based approach provided the required quantitation accuracy and precision for assay validations. Furthermore, this means that once the extraction efficiency was calibrated for a given tissue type and drug, the droplet-based approach provides a non-labor intensive and high-throughput means to acquire spatially resolved quantitative analysis of multiple samples of the same type.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2017

Robust control of a family of uncertain nonminimum‐phase systems via continuous‐time and sampled‐data output feedback

Summary The problem of global robust stabilization is studied by both continuous‐time and sampled‐data output feedback for a family of nonminimum‐phase nonlinear systems with uncertainty. The uncertain nonlinear system considered in this paper has an interconnect structure consisting of a driving system and a possibly unstable zero dynamics with uncertainty, ie, the uncertain driven system. Under a linear growth condition on the uncertain zero dynamics and a Lipschitz condition on the driving system, we show that it is possible to globally robustly stabilize the family of uncertain nonminimum‐phase systems by a single continuous‐time or a sampled‐data output feedback controller. The sampled‐data output feedback controller is designed by using the emulated versions of a continuous‐time observer and a state feedback controller, ie, by holding the input/output signals constant over each sampling interval. The design of either continuous‐time or sampled‐data output compensator uses only the information of the nominal system of the uncertain controlled plant. In the case of sampled‐data control, global robust stability of the hybrid closed‐loop system with uncertainty is established by means of a feedback domination method together with the robustness of the nominal closed‐loop system if the sampling time is small enough.

Lin, Wei↗

DOE OSTI2019

DIY XES-development of an inexpensive, versatile, and easy to fabricate XES analyzer and sample delivery system

The application of X-ray emission spectroscopy (XES) has grown substantially with the development of X-ray free-electron lasers, third and fourth generation synchrotron sources, and high-power benchtop sources. By providing the high X-ray flux required for XES, these sources broaden the availability and application of this method of probing electronic structure. As the number of sources increase, so does the demand for X-ray emission detection and sample delivery systems that are cost effective and customizable. In this work, we present a detailed fabrication protocol for von Hamos X-ray optics and give details for a 3D-printed spectrometer design. Additionally, we outline an automated, externally triggered liquid sample delivery system that can be used to repeatedly deliver nanoliter droplets onto a plastic substrate for measurement. These systems are both low cost, efficient, and easy to recreate or modify depending on the application. A low cost multiple X-ray analyzer system enables measurement of dilute samples, whereas the sample delivery limits sample loss and reproducibly replaces spent sample with fresh sample in the same position. While both systems can be used in a wide range of applications, the design addresses several challenges associated specifically with time-resolved XES (TRXES). As an example application, we show results from TRXES measurements of photosystem II, a dilute, photoactive protein.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

DOE OSTI2020

Improved sampling technique to collect natural gas from hydrate-bearing pressure cores

High quality gas compositional data are an important factor in interpreting the genetic source of natural gas hosted in hydrate-bearing sediments and other subsurface systems. In order to accurately characterize the composition of gas samples degassed from hydrate-bearing pressure cores, one must use a reproducible sampling technique that minimizes artifacts of the sampling process. Herein, we review sediment core degassing techniques and compare data obtained from a commonly used degassing approach, which we term the standard quantitative degassing (SQD) technique, to our newly developed modified quantitative degassing (MQD) method designed to minimize atmospheric contamination and gas-water interactions. The SQD method allows sample gas to interact with water in a bubbling chamber, which we hypothesize could alter the gas composition following mixing with water or dissolved gases in the bubbling chamber. Whereas, the MQD method allows for the collection of sample gas prior to the bubbling chamber. To compare the SQD and MQD methods, we performed a side-by-side comparison of noble (He, Ne, Ar, Kr, and Xe), major (H 2 , N 2 , O 2 , and CO 2 ), and hydrocarbon (CH 4 , C 2 H 6 , C 3 H 8 , i-C 4 H 10 , C 4 H 10 , i-C 5 H 12 , C 5 H 12 ) gas concentrations and select isotopic compositions obtained using both sample collection techniques. Gas samples were collected from hydrate-bearing pressure cores recovered and maintained under hydrate stable conditions from the northern Gulf of Mexico during the UT-GOM 2 -1 Expedition. The MQD method displayed significantly lower concentrations of atmospheric gases, higher proportions of hydrocarbon gases, lower ratios of C 1 /C 2 + , and heavier stable carbon and hydrogen isotopes of methane than the SQD method. These results demonstrate that the MQD method reduced air contamination and minimized alteration of the hydrocarbon gases. Finally, we conclude this method may be important for future work that seeks to determine the composition of natural gas from pressure cores using quantitative degassing experiments, especially those seeking to measure major (e.g., N 2 ) and noble gases.

58 GEOSCIENCES↗

DOE OSTI2015

Moving your laboratories to the field – Advantages and limitations of the use of field portable instruments in environmental sample analysis

The recent rapid progress in technology of field portable instruments has increased their applications in environmental sample analysis. These instruments offer a possibility of cost-effective, non-destructive, real-time, direct, on-site measurements of a wide range of both inorganic and organic analytes in gaseous, liquid and solid samples. Some of them do not require the use of reagents and do not produce any analytical waste. All these features contribute to the greenness of field portable techniques. Several stationary analytical instruments have their portable versions. The most popular ones include: gas chromatographs with different detectors (mass spectrometer (MS), flame ionization detector, photoionization detector), ultraviolet–visible and near-infrared spectrophotometers, X-ray fluorescence spectrometers, ion mobility spectrometers, electronic noses and electronic tongues. The use of portable instruments in environmental sample analysis gives a possibility of on-site screening and a subsequent selection of samples for routine laboratory analyses. They are also very useful in situations that require an emergency response and for process monitoring applications. However, quantification of results is still problematic in many cases. The other disadvantages include: higher detection limits and lower sensitivity than these obtained in laboratory conditions, a strong influence of environmental factors on the instrument performance and a high possibility of sample contamination in the field. This paper reviews recent applications of field portable instruments in environmental sample analysis and discusses their analytical capabilities. - Highlights: • Field portable instruments are widely used in environmental sample analysis. • Field portable instruments are indispensable for analysis in emergency response. • Miniaturization of field portable instruments reduces resource consumption. • In situ analysis is in agreement with green analytical chemistry principles. • Performance requirements in field analysis stimulate technological progress.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2015

Parametric models for samples of random functions

A new class of parametric models, referred to as sample parametric models, is developed for random elements that match sample rather than the first two moments and/or other global properties of these elements. The models can be used to characterize, e.g., material properties at small scale in which case their samples represent microstructures of material specimens selected at random from a population. The samples of the proposed models are elements of finite-dimensional vector spaces spanned by samples, eigenfunctions of Karhunen–Loève (KL) representations, or modes of singular value decompositions (SVDs). The implementation of sample parametric models requires knowledge of the probability laws of target random elements. Numerical examples including stochastic processes and random fields are used to demonstrate the construction of sample parametric models, assess their accuracy, and illustrate how these models can be used to solve efficiently stochastic equations.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

DOE OSTI2019

LAB4D: A low power, multi-GSa/s, transient digitizer with sampling timebase trimming capabilities

The LAB4D is a new application-specific integrated circuit (ASIC) of the Large Analog Bandwidth Recorder and Digitizer with Ordered Readout (LABRADOR) family, for use in direct wideband radio frequency digitization such as is used in ultrahigh energy neutrino and cosmic ray astrophysics. The LAB4D is a single channel switched-capacitor array (SCA) 12-bit sampler with integrated analog-to-digital converters (ADC), developed in the TSMC 0.25um process. The LAB4D, operating at 3.2GSa/s, contains 4096 total samples arranged in 32 windows, for a total record length of 1280ns. The 3dB bandwidth is approximately 1.3GHz, with a directly-coupled 50ohm input. This represents a factor of 16 increase in the sample depth and an increase in analog bandwidth and sampling depth in comparison to the previous generation LAB3 digitizer. Individually addressable windows allow for sampling and digitization to occur simultaneously, leading to nearly deadtime-free readout for kHz readout rates. All biases and current references are generated via internal digital-to-analog converters (DACs), resulting in a stand-alone digitizer with no additional support circuitry. In addition, the LAB4D contains sample cell timebase trimming capabilities, reducing the intrinsic sample-to-sample time variance to less than 5ps; an improvement of about 80%. This allows the LAB4D to be used in precision timing applications with minimal post-hoc calibration.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2015

An interface for the direct coupling of small liquid samples to AMS

We describe the moving wire interface attached to the 1-MV AMS system at LLNL’s Center for Accelerator Mass Spectrometry for the analysis of nonvolatile liquid samples as either discrete drops or from the direct output of biochemical separatory instrumentation, such as high-performance liquid chromatography (HPLC). Discrete samples containing at least a few 10 s of nanograms of carbon and as little as 50 zmol 14 C can be measured with a 3–5% precision in a few minutes. The dynamic range of our system spans approximately 3 orders in magnitude. Sample to sample memory is minimized by the use of fresh targets for each discrete sample or by minimizing the amount of carbon present in a peak generated by an HPLC containing a significant amount of 14 C. As a result, liquid sample AMS provides a new technology to expand our biomedical AMS program by enabling the capability to measure low-level biochemicals in extremely small samples that would otherwise be inaccessible.

14C↗

DOE OSTI2025

Microbiomes of frozen blood plasma samples reveal potential pathogens in wild birds and rodents

The lack of genomic data on pathogens from wildlife severely limits our ability to track transmission patterns and trace the origins of an outbreak. There are currently millions of wildlife samples in biobanks around the world, including blood samples. Blood has traditionally been viewed as a sterile environment in healthy individuals, but recent evidence suggests that this is not the case, especially for wild animals. Our goal was to determine whether frozen plasma samples can be surveyed using 16S sequencing to provide information about potential hosts for pathogens for a more complete understanding of disease systems. We sequenced blood plasma from wild North American deer mice ( Peromyscus maniculatus ) and American kestrels ( Falco sparverius ) that were cryogenically stored for 7 and 13 years, respectively, and compared two DNA extraction kits. The kestrel samples contained a very high number of reads that could not be identified to phylum compared to the mouse samples. The two kits differed in the phyla and genera that were detected, and the Zymo kit, which is optimized for plasma and serum, produced more high-quality reads for both kestrel and mouse samples. We identified several pathogenic genera, including Mycoplasma, Escherichia-Shigella , and Bartonella . Sequencing blood samples for pathogens could potentially have broad applications for identifying important reservoir hosts for pathogen transmission and provide a reduced set of species on which to follow up.

59 BASIC BIOLOGICAL SCIENCES↗

DOE OSTI2016

POF-Darts: Geometric adaptive sampling for probability of failure

We introduce a novel technique, POF-Darts, to estimate the Probability Of Failure based on random disk-packing in the uncertain parameter space. POF-Darts uses hyperplane sampling to explore the unexplored part of the uncertain space. We use the function evaluation at a sample point to determine whether it belongs to failure or non-failure regions, and surround it with a protection sphere region to avoid clustering. We decompose the domain into Voronoi cells around the function evaluations as seeds and choose the radius of the protection sphere depending on the local Lipschitz continuity. As sampling proceeds, regions uncovered with spheres will shrink, improving the estimation accuracy. After exhausting the function evaluation budget, we build a surrogate model using the function evaluations associated with the sample points and estimate the probability of failure by exhaustive sampling of that surrogate. In comparison to other similar methods, our algorithm has the advantages of decoupling the sampling step from the surrogate construction one, the ability to reach target POF values with fewer samples, and the capability of estimating the number and locations of disconnected failure regions, not just the POF value. Furthermore, we present various examples to demonstrate the efficiency of our novel approach.

97 MATHEMATICS AND COMPUTING↗