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DOE OSTI2025

Importance of Sample Handling and Preparation for Surface Analysis: A Summary of ISO Standard 20579 Part 1, Documenting and Reporting the Handling of Specimens Prior to Analysis

Reliable and reproducible analysis of surfaces is critically dependent on how samples have been collected, handled, and prepared before analysis. Although there are important, well-established general guidelines to minimize unintended alteration of the surfaces to be analyzed, specific handling steps depend on the nature of the samples and information desired. Assessments of the validity and reliability of the results require adequate information about sampling, handling, and processing. ISO standard 20579 part 1 describes the information to be recorded and reported for samples that are prepared or submitted for surface analysis. This paper summarizes elements of the standard, which includes annexes that justify and inform the sample handling processes. Also included is a checklist of information that needs to be recorded and reported and an appendix containing an example of a form that might be used to report the information.

AES↗

DOE OSTI2025

Evaluation of a high-throughput method for processing sponge-stick samples to detect viable, non-spore-forming biothreat agents

After a bioterrorism incident, surface sampling is often used to determine the extent of contamination and exposure, guiding decontamination efforts and decisions for re-occupancy of affected sites. The sponge-stick (SS) is a preferred and commonly used device for sample collection to detect both spore-forming and non-spore-forming biothreat agents from non-porous surfaces. Here, in this study, a recently developed high-throughput method (HTM) for processing SS samples to detect viable Bacillus anthracis spores was adapted for detection of non-spore-forming biothreat agents, Yersinia pestis and Francisella tularensis. The scalable HTM was used to process up to 20 SS samples simultaneously, compared to the current stomacher-based method which processes one SS at a time. Comparisons of the HTM and the stomacher-based method were statistically indistinguishable for most experiments (P > 0.05) with HTM recoveries of 37–60 % for Y. pestis inoculated at 102–103 cells/SS and held 48 h at 4 °C to mimic sample transport/storage. The HTM was integrated with Rapid Viability-Polymerase Chain Reaction (RV-PCR) analysis to detect viable Y. pestis in the presence of particulate contamination (Arizona Test Dust, ATD). This approach detected Y. pestis inoculated at 20 cells/SS and ATD did not impact detection (P > 0.05). F. tularensis showed significantly lower recoveries between no-hold time and 48-h hold time (4 °C, P < 0.05) using the HTM, which further testing showed could be due to toxicity of the neutralizing buffer used for SS pre-wetting. With modifications, this method could enhance throughput capacity while maintaining similar recovery efficiencies to current methods for other non-spore-forming bacterial pathogens.

Biological and medical sciences↗

NASA NTRS2022

Firex Water Tank, SWMU 069, Confirmatory Sampling Report: Revision 2

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 NTRS2024

Development of Cryogenic Phase Change Materials for Lunar Sample Return

One of the scientific goals of NASA’s Artemis missions is to return regolith samples from the lunar surface. To maintain scientific integrity of these samples, including any volatiles that may exist, cryogenic stowage is desired. FROSTE (Frozen Return Of Samples To Earth) is the element of the Moon to Mars architecture that is tasked with developing and advancing concepts related to this goal. Both active and passive solutions are being considered, but active solutions (cryo-coolers) have high mass and cost penalties. Phase change materials (PCMs) are commonly used as passive thermal management solutions, particularly for sensitive scientific samples. However, there are currently no PCMs capable of providing cooling at the cryogenic temperatures needed to enable lunar sample return with volatiles intact (<120 K). FROSTE has identified two possible candidate materials that could fill this gap. Testing is required to verify the thermal performance of these materials, as well as gain experience with their handling characteristics. We are conducting this testing at the Marshall Space Flight Center’s Space Environmental Effects laboratory, in vacuum, with liquid nitrogen providing cooling ability below the freezing point of the materials. In this talk, we will present an overview of the FROSTE program element and share results from the initial development testing of two cryogenic phase change materials.

phase change material↗

NASA NTRS2000

Flame Spread Along Free Edges of Thermally Thin Samples in Microgravity

The effects of imposed flow velocity on flame spread along open edges of a thermally thin cellulosic sample in microgravity were studied experimentally and theoretically. In this study, the sample was ignited locally at the middle of the 4 cm wide sample, and subsequent flame spread reached both open edges of the sample along the direction of the flow. The following flame behaviors were observed in the experiments and predicted by the numerical calculation, in order of increased imposed flow velocity: (1) ignition but subsequent flame spread was not attained, (2) flame spread upstream (opposed mode) without any downstream flame, and (3) the upstream flame and two separate downstream flames traveled along the two open edges (concurrent mode). Generally, the upstream and downstream edge flame spread rates were faster than the central flame spread rate for an imposed flow velocity of up to 5 cm/s. This was due to greater oxygen supply from the outer free stream to the edge flames and more efficient heat transfer from the edge flames to the sample surface than the central flames. For the upstream edge flame, flame spread rate was nearly independent of, or decreased gradually with, the imposed flow velocity. The spread rate of the downstream edge, however, increased significantly with the imposed flow velocity.

MICROGRAVITY↗

NASA NTRS2014

Carbon Monitoring System Flux Estimation and Attribution: Impact of ACOS-GOSAT X(CO2) Sampling on the Inference of Terrestrial Biospheric Sources and Sinks

Using an Observing System Simulation Experiment (OSSE), we investigate the impact of JAXA Greenhouse gases Observing SATellite 'IBUKI' (GOSAT) sampling on the estimation of terrestrial biospheric flux with the NASA Carbon Monitoring System Flux (CMS-Flux) estimation and attribution strategy. The simulated observations in the OSSE use the actual column carbon dioxide (X(CO2)) b2.9 retrieval sensitivity and quality control for the year 2010 processed through the Atmospheric CO2 Observations from Space algorithm. CMS-Flux is a variational inversion system that uses the GEOS-Chem forward and adjoint model forced by a suite of observationally constrained fluxes from ocean, land and anthropogenic models. We investigate the impact of GOSAT sampling on flux estimation in two aspects: 1) random error uncertainty reduction and 2) the global and regional bias in posterior flux resulted from the spatiotemporally biased GOSAT sampling. Based on Monte Carlo calculations, we find that global average flux uncertainty reduction ranges from 25% in September to 60% in July. When aggregated to the 11 land regions designated by the phase 3 of the Atmospheric Tracer Transport Model Intercomparison Project, the annual mean uncertainty reduction ranges from 10% over North American boreal to 38% over South American temperate, which is driven by observational coverage and the magnitude of prior flux uncertainty. The uncertainty reduction over the South American tropical region is 30%, even with sparse observation coverage. We show that this reduction results from the large prior flux uncertainty and the impact of non-local observations. Given the assumed prior error statistics, the degree of freedom for signal is approx.1132 for 1-yr of the 74 055 GOSAT X(CO2) observations, which indicates that GOSAT provides approx.1132 independent pieces of information about surface fluxes. We quantify the impact of GOSAT's spatiotemporally sampling on the posterior flux, and find that a 0.7 gigatons of carbon bias in the global annual posterior flux resulted from the seasonally and diurnally biased sampling when using a diagonal prior flux error covariance.

biased sampling↗

NASA NTRS2018

Low Risk Technique for Sample Acquisition from Remote and Hazardous Sites on a Comet

This paper describes a mission comet sampling strategy, known as CORSAIR (COmet Rendezvous, Sample Acquisition, Investigation, and Return), which was proposed for NASA New Frontiers 2017. The proposal was led by Applied Physics Lab (APL) with partners Goddard Space Flight Center (GSFC) and Deutsches Zentrum für Luft- und Raumfahrt (DLR). The mission concept is to launch a projectile from a satellite that is capable of gathering a 300 cc sample. The projectile is tethered and is reeled back to the spacecraft after gathering the sample. Once back at the spacecraft, a robotic manipulator extracts the sample cartridge and places the cartridge into an earth return vehicle (ERV). This method has the following favorable characteristics: 1. Places the mission at minimal risk by isolating the spacecraft from the comet 2. Allows access to remote and otherwise inaccessible locations 3. Permits deep penetration into the surface

Comet Sample↗

NASA NTRS2018

Mars Sample Return: Grand Challenge for EDL

A year ago, I gave a talk in anticipation of a Mars Sample Return effort at the 9th Ablation Workshop. Since then a lot has happened. "April of this year, after a year of study phase, NASA and ESA (European Space Agency) signed a Statement of Intent (SOI) to jointly develop a Mars Sample Return plan to be submitted to their respective authorities by the end of 2019. This signing is historic, as it signals the desire, the readiness, and the willingness to work together to execute this inspiring mission, we all have the opportunity to tackle this grand challenge. We have the scientific and engineering maturity to identify the critical technologies ready to be applied, and with discipline this campaign can be executed affordably," Jim Watzin, Mars Program Executive, NASA. NASA Centers with JPL (Jet Propulsion Laboratory) leading the charge is in the midst of a pre-formulation phase for executing a Mars Sample Return before the end of next decade. The proposed talk builds on the previous year talk. In light of the agreement between NASA and ESA, NASA has assumed the responsibilities for developing the earth entry vehicle (EEV) that will fly along with a European Spacecraft and return with the sample from Mars. EEV will be deployed for entry into earth. The EEV design, development, testing and certification have to result in a highly reliable sample return system. The entire architecture has to be demonstrated to meet the planetary protection requirement. NASA is considering two distinctly different earth entry vehicle architectures and with each choice, many different ablative TPS (Thermal Protective Shield) candidates. As a result of the NASA-ESA ongoing studies, some of the key entry conditions and design requirements are better understood today and more are being scoped out. The heat-shield ablative TPS choice need to be done with a good understanding as it plays a very significant role in determining the robustness of the EEV. Knowledge about how materials and system perform, and how the features could become flaws and how flaws lead to failure, etc. need to be clearly understood and the knowledge then need to be used to down select the TPS. This proposed talk will provide greater insight into the progress being made and the challenges that need to be tackled.

Mars Sample Return: Grand Challenge for EDL↗

NASA NTRSDate not supplied

The Stardust Sample Return Mission

The NASA Discovery-class Stardust comet sample return mission collected samples from the coma of Comet 81P/Wild 2 and returned them to Earth for study in 2006. The samples were collected at hypervelocities using low-density aerogel as the spacecraft did a flyby of the comet’s nucleus. In this talk, I will begin by giving an overview of the mission that covers (i) the mission design, (ii) the spacecraft, and (iii) the spacecraft’s encounter with Comet/81P Wild 2 and its subsequent return to Earth. This will be followed by a discussion of many of the principal scientific discoveries that resulted from both the comet flyby and the study of the returned samples in terrestrial laboratories (discoveries that will continue to grow as the returned samples continue to be studied in the future).

Comets↗

NASA NTRSDate not supplied

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↗

NASA NTRSDate not supplied

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↗

NASA NTRS2022

Firex Water Tank, SWMU 069, Confirmatory Sampling Report

Firex↗

NASA NTRSDate not supplied

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↗

NASA NTRSDate not supplied

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↗

NASA NTRSDate not supplied

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↗

NASA NTRS2024

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↗

DOE OSTI2026

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↗

DOE OSTI2024

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-↗