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At least 937 records · Page 52

Small Spacecraft Sample Return Mission Concept to Support Gateway and Lunar Science

The Lunar Gateway is a planned orbital outpost to support Lunar surface, Cislunar, and deep space exploration activities. NASA, together with international and commercial partners, are providing various capabilities, infrastructure, and services to build the Lunar economy. As Gateway capabilities and transportation logistics evolve, utilization is expected to increase, providing ample science, technology demonstration, and commercial development opportunities. Elements of the transportation network supporting Lunar activities are primarily focused on the outbound segment, which include Commercial Lunar Payload Services (CLPS), Human Landing System (HLS), Deep Space Logistics (DSL), and the SLS/Orion crew transportation system. Initially, the only Earth return segment will be provided via Orion. However, infrequent mission cadence (once every 12 months), limited payload return mass (100 kg), and operational constraints suggest that additional sample return logistics capability will be needed. Sustaining long-term presence at the Moon will likely require innovative approaches for frequent and affordable payload return. NASA Ames Research Center and the DSL team at Kennedy Space Center (which provides the Gateway Logistics Services missions) have investigated the development of a small spacecraft-based sample return capability to complement Orion. The goal of the first mission is to demonstrate the capability as a part of an early DSL mission, and provide up to 10 kg of scientific sample return from the Gateway. The mission concept envisions the progressive addition of sample return capabilities, including returning temperature- and acceleration-sensitive payloads, and evolution into a commercially provided service, similar to existing ISS payload return logistics. An overview of payload science and technology use cases and small spacecraft mission concepts will be presented to engage scientists, payload developers and mission planners who are considering Lunar exploration activities that will require the return of high-value samples from the Gateway and/or the lunar surface.

Small Spacecraft↗

Operational Workflow in a Sample Receiving Facility: Input from the MSR Operation Definition Team

The return of scientifically selected samples from Mars would provide a rare opportunity for investigation with the full range of the latest technology available. To take full advantage of this opportunity, it is important to plan ahead to ensure the pristine nature of the samples upon arrival within the Earth environment until scientific investigations can begin. The NASA/ESA science community-driven MSR Science Planning Group – Phase 2 (MSPG2) delivered recommendations and guidance regarding curation (1) and science (2,3) activities to be performed on the samples under containment. High-level requirements for the infrastructure were also developed by MSPG2 (4). In order to prepare infrastructure-targeted input for the ESA and NASA facility studies planned in the 2022-2023 timeframe, the MSR agency-led Operational Scenarios Definition Team (MOSDT) was assembled to conceptualize the sample operations that will inform future architecture teams. Emphasis was placed on the responsibility of MOSDT to use community-defined requirements and to represent the view of the international scientific community. The main deliverable of MOSDT was an operational workflow for a Sample Receiving Facility (SRF). Two other deliverables were produced: a report to narrate the workflow, and a list of instruments (see Hutzler et al., this conference). Activities described in the main sequence of the workflow range from engineering operations to curation to science, with the latter term being used here as the science to be done within a SRF. Side sequences (e.g. engineering inspection of hardware, head gas extraction) were also identified, and detailed when they would have a significant impact on the infrastructure of a SRF. It was necessary for the MOSDT to rely on assumptions for some steps and activities, and though these were kept to a minimum (and are described in both the report supporting the workflow and in the full presentation), in general, the assumptions and overall work were very conservative, as the impact of underestimating the scope of the SRF infrastructure was considered more detrimental than overestimating it. It is expected that future work will be able to confirm or inform these assumptions. The community was consulted during the course of the MOSDT work. This abstract’s aim is two-fold: on one hand, inform the scientific community and overall MSR stakeholders, to make the infrastructure studies and trade-off more understandable; on the other hand, to solicit feedback from a larger community audience for the next iterations planning for SRF design and activities.

Mars Sample Return↗

Firex Water Tank, SWMU 069, Confirmatory Sampling Report

The National Aeronautics and Space Administration (NASA) Resource Conservation and Recovery Act (RCRA) permit requires identification and evaluation of known Solid Waste Management Units (SWMU) located at the Kennedy Space Center (KSC). Firex Water Tank (FWT), or the “site,” is designated as SWMU 069 under the NASA RCRA permit. This report summarizes the results of the Confirmatory Sampling (CS) field activities carried out during Fall 2021, at FWT, SWMU 069, KSC, Florida. Three locations of concern (LOCs) were identified by screening historical sample results to current State of Florida soil cleanup target levels (SCTL). A total of 18 soil samples were collected to investigate the historical exceedance locations. Samples at LOC 1 and 2 were analyzed for arsenic and the results for all were below the SCTL. Samples at LOC 3 were analyzed for polynuclear aromatic hydrocarbons and it was determined that certain locations have results that remain above the SCTL. The current land use controls will remain in place at FWT to mitigate potential risks.

Firex↗

NASA Capture, Containment, and Return System: Bringing Mars Samples to Earth

The Capture, Containment, and Return System (CCRS) project is NASA’s last step in bringing back Mars samples. CCRS will close a decades-long multi-mission and multi-agency effort to bring Mars surface samples back to Earth for scientific studies. CCRS will launch in 2027 on the European Earth Return Orbiter (ERO) spacecraft, which will provide communications relay for the Mars Sample Return ground missions, Perseverance rover and the Sample Retrieval Lander (SRL) (to be launched in 2028). The main mission for CCRS begins when the first-ever orbital planetary capture operation occurs with CCRS catching and securing the Orbiting Sample (OS)in low Mars orbit. From this point, the system will perform additional "firsts": it will autonomously contain the OS with heat-shrink-fit, sterilize the outside surface, and assemble the Earth entry capsule, named Earth Entry System (EES), in orbit around Mars using a gantry mechanism. At approximately 2.8 Lunar distances from Earth, or 3-days from entry into Earth’s atmosphere, CCRS will open its micrometeoroid shield and release the EES on a ballistic trajectory to Earth. The EES is designed to be a fully passive system that will enter the atmosphere and land without parachute at the Utah Test and Training Range (UTTR).

Mars mission, Sample return, Mission design↗

On-ground Live Fuel Moisture Content Sampling Along California’s Central Coast Santa Lucia Preserve - Carmel Valley, CA

The ratio of water to dry mass within live plants is an important factor when determining the severity and intensity of potential wildfires. Currently, live fuel moisture content (LFMC) samples support wildland fire management, but are limited in number and spatial extent. In Monterey County, the only LFMC data to analyze spatial and temporal trends is collected by CalFire and the Los Padres National Forest Unit of the United States Forest Service across five long-term sampling sites. Our project aims to enhance the spatial coverage of current LFMC data being collected across Monterey County. Here, we share results from the ongoing work to monitor LFMC across Carmel Valley, CA. We evaluate LFMC data by environmental factors such as slope, aspect, topography, and species composition. We also place our LFMC samples in relation to nearby long-term sampling locations. We conclude by interpreting spatial and temporal trends in the preliminary data and discuss logistical challenges of establishing more long-term LFMC sampling sites to better represent the complex topography and vegetation composition of Central California.

On-ground↗

Genesis Solar Wind Sample Curation Facility

The controlled access facility designed and constructed for storing and examining Genesis solar wind samples consists of two adjacent laboratories, both ISO Class 4 cleanrooms (vertical laminar flow, ULPA filtered). One cleanroom is equipped with ultrapure water (UPW) for experimental cleaning of containers and tools used in handling the solar wind samples, flight hardware and witness plates. The ultrapure water is also used for cleaning the solar wind samples. The other cleanroom is for long-term nitrogen storage of samples and for examination and processing of Genesis samples.

Curation Facility↗

Key Perseverance Sampling Locations for the Ancient Martian Crust and Implications for Mars Science

Since Feb 2021, the Perseverance rover has collected samples in the Jezero crater. The plan baselined at the 2018 landing site selection, subsequently further developed by the Mars-2020 team, and presented to the Decadal Survey included the exploration and sampling of the Jezero crater rim and the Nili Planum area, a rock record that is important to preserving the science return of the endeavor. Specifically, the science team identified the following prioritized science objectives aligned with community objectives that are not covered by the current sample cache: 1) Investigate the habitable environments with potential biosignatures from a more ancient time interval and from a diverse set of geological environments (incl. exposed subsurface) than the Jezero crater sedimentary deposits (Fig. 2). (2) Determine radioisotopic ages for well-defined craterretaining surfaces and/or the Isidis basin impact event. (3) Characterize ancient aqueous environments to study climate, environmental transitions, and habitability on ancient Mars. (4) Investigate planetary accretion, crustal evolution, and dynamo activity through analysis and sampling of igneous lithologies. (5) Study the geology of basin-forming impacts. In addition, for the Jezero rim and any Jezero ejecta: (6) Analyze Jezero impactites for potentially habitable hydrothermal environments and radioisotopic dating of the Jezero crater formation. From 2018 to now, we used a combination of High Resolution Imaging Experiment (HiRISE) and Compact Reconnaissance Imaging Spectrometer for Mars (CRISM) data to further characterize Jezero rim and Nili Planum, culminating in our prioritized sample location recommendations: (1) Monument Valley and (2) Northwest Jezero rim.

Mars sample return↗

Improvement of Drop‐Hammer Impact Testing for Safety Assessment of High Explosives Using 10‐mg Samples

Here, in this study, we established an improved method for drop-hammer impact testing of small quantities of high explosives (10 mg). We performed about seven hundred impact tests under various experimental conditions (e.g., sandpaper vs bare anvil, different sample masses, drop-weights, and striker diameters) to determine an optimal set of conditions and reaction detection methods (e.g., gas analysis, video, and sound recordings) that give the most statistically reliable results with 10 mg samples. We used both Frequentist and Bayesian statistical approaches to compare estimates of the drop height (DH50) that initiates a reaction 50% of the time, and to quantify the associated uncertainty. Gas analysis proved to be the most reliable reaction detection method, showing unambiguous rises in HE decomposition products (e.g., CO 2 ) even when the other indicators (e.g., sound, video) were inconclusive. The impact tests performed with a bare anvil showed much better reproducibility than those conducted with sandpaper, reducing the largest uncertainty observed in the data sets by a factor of 1.7. The DH 50 values obtained from three different sample masses (10, 20, and 35 mg) fell within the uncertainties of the measurements. We demonstrated the improved procedure (i.e., 10-mg samples, gas analysis, bare anvil, and Bayesian approach) on a variety of PETN samples having different surface areas and thermal histories.

PETN↗

Robust surfactant-assisted one-pot sample preparation for label-free single-cell and nanoscale proteomics

With advanced mass spectrometry (MS)-based proteomics, genome-scale proteome coverage can be achieved from bulk cells. However, such bulk measurement obscures cell to cell heterogeneity, precluding proteome profiling of single cells and small numbers of cells of interest. To address this issue, in recent 5 years there are a surge of small sample preparation methods developed for robust effective collection and processing of single cells and small numbers of cells for in-depth MS-based proteome profiling. Based on their broad accessibility, they can be categorized into two types: specific device- and standard PCR tube- or multi-well plate-based methods. Herein we describe the detailed protocol of our recently developed, easily adoptable, Surfactant-assisted One-Pot (SOP) sample preparation coupled with MS method termed SOP-MS for label-free single-cell and nanoscale proteomics. SOP-MS capitalizes on the combination of a MS-compatible surfactant, DDM (n-Dodecyl-ß-D-maltoside), and standard low-bind PCR tube or multi-well plate for ‘all-in-one’ one-pot sample preparation without sample transfer. With its robust and convenient features, SOP-MS can be readily implemented in any MS laboratory for single-cell and nanoscale proteomics. With further improvements in MS detection sensitivity and sample throughput, we believe that SOP-MS could open an avenue for single-cell proteomics with broad applicability in the biological and biomedical research.

Single-cell proteomics, nanoscale proteomics, SOP-↗

Evaluation of dried blood spot sampling for verification of exposure to chemical threat agents

Abstract Purpose Exposure to chemical threat agents (CTAs), including nerve agents, the vesicating agent sulfur mustard, and opioids, remains a significant threat to warfighter and civilian populations. Definitive analytical methods to verify exposure to CTAs require shipping refrigerated or frozen biomedical samples to reference laboratories for analysis. Logistical and financial burdens arise as the transport of biomedical samples is subject to strict restrictions and complex packaging, which, if done incorrectly, can lead to sample deterioration. The use of dried blood spot (DBS) sampling could provide operational improvements for collecting, storing, and shipping important forensic samples. Therefore, this effort focuses on developing DBS techniques with Mitra® 30-µL volumetric absorptive microsampling (VAMS®) devices for use in CTA exposure verification. Methods VAMS® devices were loaded and dried with human whole blood that was exposed to the metabolites pinacolyl methylphosphonic acid (PMPA), ethyl methylphosphonic acid (EMPA), 1,1’sulfonylbis[2-(methylsulfinyl)ethane] (SBMSE), norfentanyl, norcarfentanil, norsufentanil, and norlofentanil. Following extraction from the VAMS® devices, metabolites were detected using liquid chromatography-tandem mass spectrometry (LC–MS/MS). The methods were validated for performance by assessing sensitivity, precision, accuracy, and recovery. Results These methods were sensitive to 1 ng/mL for SBMSE, 0.5 ng/mL for PMPA, EMPA, and norfentanyl; 0.1 ng/mL for norlofentanil, and 0.05 ng/mL for norsufentanil and norcarfentanil. All methods met acceptable precision and accuracy criteria with favorable recovery. Conclusions These results demonstrated the utility of VAMS® in stabilizing human whole blood and show promise as an improved collection method for verification of exposure to various CTAs.

Toxicology↗

Sampling two-dimensional isometric tensor network states

Sampling a quantum system’s underlying probability distributions is an important computational task, e.g., for quantum advantage experiments and quantum Monte Carlo algorithms. Tensor networks are an invaluable tool for efficiently representing states of large quantum systems with limited entanglement. Algorithms for sampling one-dimensional (1D) tensor networks are well-established and utilized in several 1D tensor network methods. In this paper we introduce two novel sampling algorithms for two-dimensional (2D) isometric tensor network states (isoTNS) that generalize existing 1D tensor network sampling algorithms. Our first proposed algorithm performs independent sampling and yields a single configuration together with its associated probability. The second algorithm employs a greedy search strategy to identify high-probability configurations and their corresponding probabilities. Numerical results demonstrate the effectiveness of these algorithms across quantum states with varying entanglement and system size.

Dumitrescu, Eugene [ORNL] (ORCID:0000000158519567)↗

Spatially Resolved Top-Down Proteomics of Tissue Sections Based on a Microfluidic Nanodroplet Sample Preparation Platform

Conventional proteomics measures the averaged signal from mixed cell populations or bulk tissues, leading to the dilution of significant changes in subpopulations of cells that might serve as important biomarkers. Recent developments in bottom-up proteomics have enabled spatial mapping of cellular heterogeneity in tissue microenvironments. However, bottom-up proteomics cannot precisely infer the abundance changes of intact proteins, which are presented as proteoforms. Herein, we described a spatially resolved top-down proteomics (TDP) platform for proteoform identification and quantification directly on thin tissue sections. The spatial TDP platform consisted of a nanoPOTS (nanodroplet Processing in One pot for Trace Samples)-based sample preparation system and an LCM (laser capture microdissection)-based cell isolation system. We improved the nanoPOTS sample preparation by adding benzonase in the extraction buffer to enhance the coverage of nucleus proteins. Using ~200 cultured cells as model samples, the improved approach increased proteoform identifications from 493 to 700; newly identified proteoforms primarily corresponded to nuclear proteins. To demonstrate the spatial TDP platform in tissue samples, we analyzed LCM-isolated tissue voxels from rat brain cortex and hypothalamus regions. We quantified 426 proteoforms by combining identifications from TopPIC and TDPortal with the quantitation from ProMex. Several proteoforms corresponding to the same gene exhibited mixed abundance profiles between two tissue regions, suggesting potential PTM-specific spatial distributions. The spatial TDP workflow has prospects for biomarker discovery at proteoform level from small tissue sections.

59 BASIC BIOLOGICAL SCIENCES↗

A machine-learning approach to measure 3D sample properties from 2D Transmission Electron Microscopy images

Transmission Electron Microscopy (TEM) is a powerful tool for the characterization of materials at the nanoscale; however, its inherent two-dimensional (2D) nature poses significant challenges to accurately measure three-dimensional (3D) properties. We introduce a supervised machine-learning model that predicts 3D structural information, such as sample thickness and curvature, from a series of conventional 2D TEM images. The model, a U-Net convolutional neural network, is trained on a large synthetic dataset generated from dynamical diffraction simulations that model TEM’s complex, nonlinear image formation, accounting for sample thickness and curvature. This physically realistic framework enables exploration of a broad parameter space impractical to sample experimentally. We demonstrate that the trained model has accurate predictions for experimental single-crystal silicon samples, achieving performance comparable to established measurement techniques. This work highlights the critical role of robust, simulation-based training in overcoming the limitations of real-world imaging artifacts and inconsistent sample geometries. By integrating machine learning with numerical simulations, we offer an efficient and scalable framework for quantitative TEM analysis, paving the way for more sophisticated 3D characterization of complex materials.

Dynamical diffraction↗

Proof-of-concept chemometric approach for environmental forensic sourcing of crude oil samples using SPME-GC-MS

Environmental exposure to crude oil through seepage and spillage poses risks to the immediate environment and the broader ecosystem as areas along the oil distribution path are affected by the influx of crude petroleum as well as the environmental, economic, and civil unrest that accompanies it. There is a large financial burden associated with the lost resources, including the cost of rehabilitation, and the affected sources of revenue for communities affected by oil spills. As such, it is crucial to determine the responsible parties. This work outlines an environmental forensics approach to determining the source of an un-weathered crude oil sample. The researchers employed solid phase microextraction coupled with gas chromatography mass spectrometry (SPME-GC-MS) to capture and analyze the gaseous components emitted by crude oil samples sourced from five locations. Samples were analyzed using Spearman's rank correlation and 3D covariance analysis. Both chemometric approaches yielded optimal performance results with no misclassifications, true positive rate (TPR) = 100 % and false positive rate (FPR) = 0 %. The similarity metrics calculated by each test noted clear delineations between the values of same-source and differently sourced samples. The Spearman's rank correlation test and 3D covariance calculations both demonstrated the ability to correctly identify sample source origin in this dataset. Finally, the authors outline an approach to the future application of these tests and suggest their joint use in future crude oil sourcing endeavors.

3D covariance mapping↗

Quantifying Phospholipids in Organic Samples Using a Hydrophilic Interaction Liquid Chromatography–Inductively Coupled Plasma High-Resolution Mass Spectrometry (HILIC-ICP-HRMS) Method

Here, in this study, a novel method using hydrophilic interaction liquid chromatography (HILIC) coupled with inductively coupled plasma high-resolution mass spectrometry (ICP-HRMS) was introduced for the quantification of phospholipids in oil samples. The method employed a bridged ethyl hybrid (BEH) stationary phase HILIC column with a tetrahydrofuran (THF)/water mobile phase, enhancing the solubility and detection of phospholipids. During the study, a gradient/matrix effect on ICP-HRMS sensitivity was observed and successfully compensated for experimentally, ensuring reliable quantification results. This approach has proven effective for a wide range of different oil samples including vegetable oils, animal fats, and phospholipid supplements. Notably, this method allowed the direct quantification of phospholipids in oil samples, bypassing the need for prior sample preparation methods, such as solid phase extraction (SPE), thereby streamlining the analytical process. The precision, accuracy, and reduced need for extensive sample preparation offered by this method mark a significant advancement in lipids analysis. Its robustness and broad applicability have substantial implications for industries such as food and renewable energy production, where both efficient and accurate lipid identification and quantification are crucial.

09 BIOMASS FUELS↗

Single-Particle Isotopic Analysis Using the Liquid Sampling-Atmospheric Pressure Glow Discharge Microplasma Coupled to an Orbitrap Mass Spectrometer

Isotope ratio (IR) determinations on individual particles can provide valuable information relative to the sample, including processing and dating, which could be valuable to geological and nuclear material analysis communities. In comparison to “bulk” measurements, in which all particle information is lost and homogenized within a sample, “particle” measurements allow for fingerprinting and can provide unique insights related to the sample’s nano- and micro- compositions. Furthermore, the complex nature of particles, with potential isobaric interferences from either the matrix or other elements within the same particle, poses a significant analytical challenge for conventional mass spectrometry platforms employed for elemental analysis due to their limited mass resolution. Presented here is the first demonstration of an ultrahigh resolution method for single particle (SP) isotopic analysis using the liquid sampling-atmospheric pressure glow discharge (LS-APGD) microplasma ionization source coupled to an Orbitrap mass spectrometer and FTMS Booster X2T acquisition/processing system. For proof of concept, well-characterized CeO 2 microparticles with a nominal diameter of 1.0 μm were analyzed at a mass resolution of ∼330,000. Important instrumental parameters were optimized to enable the detection of single particles. The 142 Ce/ 140 Ce ratio of individual particles and the population average were determined and compared to an SP inductively coupled plasma time-of-flight mass spectrometry (ICP-TOF-MS) analysis. The isotopic accuracy and precision were determined by two methods and found to be in good agreement with the SP-ICP-TOF-MS method, with the linear regression slope method providing a more accurate ratio, showing a ∼1.4% relative difference from the ratio determined from a particle digest. The encouraging performance of the method was further supported by a determined detection limit of 2.9 fg ( 142 Ce). The developed method is anticipated to overcome many of the challenges posed by isobaric interferences encountered in conventional mass spectrometry techniques when analyzing real-world samples for particle isotopic composition.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Sample Preparation Methods for Targeted Single-Cell Proteomics

We compared three cell isolation and two proteomic sample preparation methods for single-cell and near-single-cell analysis. Whole blood was used to quantify hemoglobin (Hb) and glycated-Hb (gly-Hb) in erythrocytes using targeted mass spectrometry and stable isotope-labeled standard peptides. Each method differed in cell isolation and sample preparation as follows: 1) FACS and automated preparation in one-pot for trace samples (autoPOTS); 2) limited dilution via microscopy and a novel rapid one-pot sample preparation method that circumvented the need for the solid-phase extraction, low-volume liquid handling instrumentation and humidified incubation chamber; and 3) CellenONE-based cell isolation and the same one-pot sample preparation method used for limited dilution. Only the CellenONE device routinely isolated single-cells from which Hb was measured to be 540–660 amol per red blood cell (RBC), which was comparable to the calculated SI reference range for mean corpuscular hemoglobin (390–540 amol/RBC). FACSAria sorter and limited dilution could routinely isolate single-digit cell numbers, to reliably quantify CMV-Hb heterogeneity. Finally, we observed that repeated measures, using 5–25 RBCs obtained from N = 10 blood donors, could be used as an alternative and more efficient strategy than single RBC analysis to measure protein heterogeneity, which revealed multimodal distribution, unique for each individual.

59 BASIC BIOLOGICAL SCIENCES↗

Sparge Sampling of Molten Salts for Online Monitoring via Laser-Induced Breakdown Spectroscopy

A method was developed to sample molten salts by sparging to generate and transport aerosols to an isolated instrument for compositional analysis by laser-induced breakdown spectroscopy (LIBS). Real-time monitoring of molten salt composition is critical to developing molten salt nuclear reactors, which offer enhanced safety and efficiency. In this article, the sparge sampling method is described and compared with sampling using a Collison nebulizer. The size distribution and transport of aerosols produced from molten eutectic NaNO 3 –KNO 3 salt were compared for multiple gas flow rates (75–1200 mL min –1 ) and transport distances (0.68–2.61 m). Both methods produced aerosols ranging from 0.5 to 5.0 μm determined using a cascade impactor. Aerosols were effectively transported without pre- or trace-heating of gas lines, but transport efficiency was reduced by the formation of agglomerates. Sparge sampling was found to use less sample and less gas than a Collison nebulizer while producing a more concentrated aerosol stream (up to 5 μg L –1 ). The effects of laser energy and delay time on the signal quality of LIBS measurements of these aerosols were also studied. High energy and short delay times were found to enhance signal and repeatability, whereas signal-to-background and signal-to-noise ratios were highest at low energy and longer delay times. The capabilities of this system for online monitoring of molten salts were demonstrated with calibrations for Sr and Li with relative standard deviations of 2.6% and 1.5% and limits of detection of 380 and 180 μg g –1 , respectively.

Aerosols↗