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Synchronous Separation, Seaming, Sealing and Sterilization (S4) using Brazing for Sample Containerization and Planetary Protection

The return of samples back to Earth in future missions would require protection of our planet from the risk of bringing uncontrolled biological materials back with the samples. This protection would require “breaking the chain of contact (BTC)”, where any returned material reaching Earth for further analysis would have to be sealed inside a container with extremely high confidence. Therefore, the acquired samples would need to be contained while destroying any potential biological materials that may contaminate the external surface of the container. A novel process that could be used to contain returning samples has been developed and demonstrated in a quarter scale size. The process consists of brazing using non-contact induction heating that synchronously separates, seams, seals and sterilizes (S4) the container. The use of brazing involves melting at temperatures higher than 500°C and this level of heating assures sterilization of the exposed areas since all carbon bonds (namely, organic materials) are broken at this temperature. The mechanism consists of a double wall container with inner and outer shells having Earth-clean interior surfaces. The process consists of two-steps, Step-1: the double wall container halves are fabricated and brazed (equivalent to production on Earth); and Step-2 is the S4 process and it is the equivalent to the execution on-orbit around Mars. In a potential future mission, the double wall container would be split into two halves and prepared on Earth. The potential on-orbit execution would consist of inserting the orbiting sample (OS) container into one of the halves and then mated to the other half and brazed. The latest results of this effort will be described and discussed in this manuscript.

Salazar, Eduardo↗

Self-Sealing Wet Chemistry Cell for Field Analysis

In most analytical investigations, there is a need to process complex field samples for the unique detection of analytes, especially when detecting low concentration organic molecules that may identify extraterrestrial life. Wet chemistry based instruments are the techniques of choice for most laboratory- based analysis of organic molecules due to several factors including less fragmentation of fragile biomarkers, and ability to concentrate target species resulting in much lower limits of detection. Development of an automated wet chemistry preparation system that can operate autonomously on Earth and is also designed to operate under Martian ambient conditions will demonstrate the technical feasibility of including wet chemistry on future missions. An Automated Sample Processing System (ASPS) has recently been developed that receives fines, extracts organics through solvent extraction, processes the extract by removing non-organic soluble species, and delivers sample to multiple instruments for analysis (including for non-organic soluble species). The key to this system is a sample cell that can autonomously function under field conditions. As a result, a self-sealing sample cell was developed that can autonomously hermetically seal fines and powder into a container, regardless of orientation of the apparatus. The cap is designed with a beveled edge, which allows the cap to be self-righted as the capping motor engages. Each cap consists of a C-clip lock ring below a crucible O-ring that is placed into a groove cut into the sample cap.

Beegle, Luther W.↗

Lunar rock splitter/can sealer

A manually powered and operated force generating device fractures lunar material as received from the moon and seals cans containing lunar samples. The rock splitting and can sealing operations are carried out in a vacuum environment. Can sealing is a cold welding process that requires a pressure of 125,000 psi (generating 32,000 lb for the largest can used). The design and modification of the device and the operating experience are described.

Johnson, K. G.↗

Impact of Drilling Operations on Lunar Volatiles Capture: Thermal Vacuum Tests

In Situ Resource Utilization (ISRU) enables future planetary exploration by using local resources to supply mission consumables. This idea of 'living off the land' has the potential to reduce mission cost and risk. On the moon, water has been identified as a potential resource (for life support or propellant) at the lunar poles, where it exists as ice in the subsurface. However, the depth and content of this resource has yet to be confirmed on the ground; only remote detection data exists. The upcoming Resource Prospector mission (RP) will 'ground-truth' the water using a rover, drill, and the RESOLVE science package. As the 2020 planned mission date nears, component level hardware is being tested in relevant lunar conditions (thermal vacuum). In August 2014 a series of drilling tests were performed using the Honeybee Robotics Lunar Prospecting Drill inside a 'dirty' thermal vacuum chamber at the NASA Glenn Research Center. The drill used a unique auger design to capture and retain the lunar regolith simulant. The goal of these tests was to investigate volatiles (water) loss during drilling and sample transfer to a sample crucible in order to validate this regolith sampling method. Twelve soil samples were captured over the course of two tests at pressures of 10(exp-5) Torr and ambient temperatures between -80C to -20C. Each sample was obtained from a depth of 40 cm to 50 cm within a cryogenically frozen bed of NU-LHT-3M lunar regolith simulant doped with 5 wt% water. Upon acquisition, each sample was transferred and hermetically sealed inside a crucible. The samples were later baked out to determine water wt% and in turn volatile loss by following ASTM standard practices. Of the twelve tests, four sealed properly and lost an average of 30% of their available water during drilling and transfer. The variability in the results correlated well with ambient temperature (lower the temperature lower volatiles loss) and the trend agreed with the sublimation rates for the same temperature. Moisture retention also correlated with quantity of sample: a larger amount of material resulted in less water loss. The drilling process took an average of 10 minutes to capture and transfer each sample. The drilling power was approximately 20 Watt with a Weight on Bit of approximately 30 N. The bit temperature indicated little heat input into formation during the drilling process.

drilling↗

Low-closing-force seal

Compress soft, inert metal gasket between cone and corresponding socket to attach tubes to vessels containing gas samples. Technique effects seals with minimum of applied force and does not contaminate contents. Seal is formed when port connector is pushed firmly into its socket. Gold washer is deformed and forced to flow into imperfections in surfaces.

Bergquist, L. E.↗

Thermal Analysis of Brazing Seal and Sterilizing Technique to Break Contamination Chain for Mars Sample Return

The potential to return Martian samples to Earth for extensive analysis is in great interest of the planetary science community. It is important to make sure the mission would securely contain any microbes that may possibly exist on Mars so that they would not be able to cause any adverse effects on Earth's environment. A brazing sealing and sterilizing technique has been proposed to break the Mars-to-Earth contamination chain. Thermal analysis of the brazing process was conducted for several conceptual designs that apply the technique. Control of the increase of the temperature of the Martian samples is a challenge. The temperature profiles of the Martian samples being sealed in the container were predicted by finite element thermal models. The results show that the sealing and sterilization process can be controlled such that the samples' temperature is maintained below the potentially required level, and that the brazing technique is a feasible approach to break the contamination chain.

Bao, Xiaoqi↗

The Collection, Usage, and Preliminary Examination of the Apollo Sample Suite: Lessons for Artemis

Apollo Sample Collection and Usage: From 1969 to 1972 there were six Apollo missions to the surface of the Moon during which the astronauts collected 382 kg of rock and regolith (~2200 samples). The samples collected fall into these general categories: rocks (~66% by mass), rake samples (~4%), bulk regolith (~24%), and specialty regolith (deep drill cores, drive tubes, sealed bulk regolith) samples (~6%). In each category there are a variety of different subtypes available for study, e.g., among the bulk regolith samples there are also skim, trench, and (partially) shaded regolith samples each sampling unique types or depths of regolith. This variety of subsamples has enabled a multitude of different studies over the past 55 years (>3400 individual requests). We are still averaging ~50 unique requests and have allocated >500 individual Apollo samples annually for the past 10 years (2020 excepted). Looking at the 4,675 non-ANGSA (Apollo Next Generation Sample Analysis) samples allocated over the past 10 years, the proportions of allocated samples do not precisely align with the abundance (by mass) of those samples withing the collection: Rock (69.4 %); Rake (10.8 %); Bulk Regolith (15.5 %); Drive Tube (3.3 %); Core/Specialty (1.0 %). Apollo Preliminary Examination (PE): The PE process differs significantly for the various sample types enumerated above; we focus on regolith and rock samples here. During the Apollo mission era, the PE process evolved over the course of the missions; below is what was done for the Apollo 17 mission. For regolith samples, the PE process was: (1) documented bags containing regolith are opened, photographed, and described; (2) large rocks are removed and treated separately; (3) 25% to 33% of the bulk soil is scooped out, weighed, and stored in reserve; (4) the remaining sample is sieved to produce the size fractions <1, 1- 2, 2-4, and 4-10 mm, all of which are weighed. For rock samples, the process is: (1) removing rocks from the container(s) it came back from the Moon in; (2) rematching any materials that spalled off the rock to their original location; (3) numbering, weighing, and basic photographic documentation; (4) dusting with a gentle N2 gas jet; (5) Orthogonal photography; (6) detailed description of the textures and features of the rock; (7) rock modelling and measurement; (8) stereophotography; (9) determination of the orientation of the rock on the lunar surface. Drive tubes and deep drill cores were not characterized during PE beyond an initial weight and a sketch of the interior tube materials derived from 2D medical X-ray images. Catalogs: The ongoing utility of the Apollo samples is enabled by the robust cataloguing process for the samples [3-5], which allows the scientific community to accurately request samples uniquely suited to their proposed studies. A common misconception, however, is the amount of detail that goes into the initial catalog (e.g., [6]) for a collection from the preliminary examination (PE) period, versus what goes into the catalogs that come later in the life cycle of the samples from that mission (e.g., [7]). The only required data for a PE catalog is a weight, a basic photograph, and a description of the nature of the sample. Artemis PE: Over the past few years, the ongoing ANGSA project studied previously unopened Apollo 17 double drive tube samples 73001/2 [1], and a PE of the drive tubes was done. The PE took the existing core dissection process (developed during PE of Apollo cores in the 1970s, 1980s), and modernized it [7]. The main lesson from the ANGSA PE relative to future missions was that the physical work done during PE of lunar samples has not changed much over the past 5 decades. The use of “modern” technology during PE (e.g., XCT; multispectral analyses) resulted in an enhanced initial understanding of the 73001 and 73002 drive tubes, but greatly increased the time required. The lessons learned from recent astromaterial PEs (e.g., ANGSA and OREx) are important to consider when planning for Artemis, but the unique nature of the Artemis Campaign means many lessons learned from these mission will not be applicable. Given the time constraints (6 months) and likely number of samples that will be returned by Artemis (>200), the Artemis PE catalog will necessarily look much more like [4] than [6].

J Gross↗

The Mars Sample Return Analogue Collection

The Mars 2020 Perseverance rover touched down in Jezero crater on February 18th, 2021, and sealed the first sample for Mars Sample Return (MSR) later that summer. As of sol 1088, 23 rock cores have been collected across a diverse set of lithologies that span rock types from sedimentary to igneous. As the cache on Perseverance continues to grow, the overall portfolio of MSR expands, creating long lasting implications for a wide net in the scientific community as well as supporting detailed analyses for generations to come. To best prepare for these precious samples to return to Earth one day, NASA and ESA are jointly planning to create a MSR Analogue Collection that will be available to the community in the near future.

M T Thorpe↗

Progress Report on Graphite-Salt Interaction Studies (FY21)

This report summarizes the activities performed in FY21 to investigate the interactions between nuclear graphite and molten salts, such as FLiNaK. First, building on last year’s achievements, the team improved the procedure for measurements on pressurized salt intrusion in nuclear graphite and performed new experiments at variable pressures with specimens of different sizes and shapes. Additionally, the team actively provided suggestions and comments for ASTM D8091, Standard Guide for Impregnation of Graphite with Molten Salts , which came up for periodic revision in 2021. Second, the team expanded its capabilities to further characterize salt-impregnated graphite by procuring and installing a laser-induced breakdown spectroscopy (LIBS) instrument capable of producing a 3D chemical composition of a surface and subsurface region of specimens. A methodology for accurately analyzing information was developed, and a manuscript was submitted for publication. The LIBS instrument sample cell is sealed in controlled inert atmosphere, which is an advantage for using humidity-sensitive samples and Be-contaminated samples. This aligns with the team’s effort to expand the capabilities of handling FLiBe and Becontaining materials in two newly installed glovebox units. Third, the team performed preliminary tribology tests for pebble graphite wear in contact with stainless steel in dry state and in molten salt at high temperature. These tests are needed to establish the baseline for the wear of pebble graphite by friction against metallic walls. The friction and wear of pebbles in the fluoride salt-cooled hightemperature reactor are expected to generate dust, which is a concern for other components’ properties and safe reactor operation.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

International Agreement on Planetary Protection

The maintenance of a NASA policy, is consistent with international agreements. The planetary protection policy management in OSS, with Field Center support. The advice from internal and external advisory groups (NRC, NAC/Planetary Protection Task Force). The technology research and standards development in bioload characterization. The technology research and development in bioload reduction/sterilization. This presentation focuses on: forward contamination - research on the potential for Earth life to exist on other bodies, improved strategies for planetary navigation and collision avoidance, and improved procedures for sterile spacecraft assembly, cleaning and/or sterilization; and backward contamination - development of sample transfer and container sealing technologies for Earth return, improvement in sample return landing target assessment and navigation strategy, planning for sample hazard determination requirements and procedures, safety certification, (liaison to NEO Program Office for compositional data on small bodies), facility planning for sample recovery system, quarantine, and long-term curation of 4 returned samples.

Source record↗

Biofilm monitoring coupon system and method of use

An apparatus and method is disclosed for biofilm monitoring of a water distribution system which includes the mounting of at least one fitting in a wall port of a manifold in the water distribution system with a passage through the fitting in communication. The insertion of a biofilm sampling member is through the fitting with planar sampling surfaces of different surface treatment provided on linearly arrayed sample coupons of the sampling member disposed in the flow stream in edge-on parallel relation to the direction of the flow stream of the manifold under fluid-tight sealed conditions. The sampling member is adapted to be aseptically removed from or inserted in the fitting and manifold under a positive pressure condition and the fitting passage sealed immediately thereafter by appropriate closure means so as to preclude contamination of the water distribution system through the fitting. The apparatus includes means for clamping the sampling member and for establishing electrical continuity between the sampling surfaces and the system for minimizing electropotential effects. The apparatus may also include a plurality of fittings and sampling members mounted on the manifold to permit extraction of the sampling members in a timed sequence throughout the monitoring period.

Sauer, Richard L.↗

Application of Pinniped Vibrissae to Aeropropulsion

Vibrissae of Phoca Vitulina (Harbor Seal) and Mirounga Angustirostris (Elephant Seal) possessundulations along their length. Harbor Seal Vibrissae were shown to reduce vortex induced vibrations and reduce dragcompared to appropriately scaled cylinders and ellipses. Samples of Harbor Seal vibrissae, Elephant Seal vibrissae andCalifornia Sea Lion vibrissae were collected from the Marine Mammal Center in California. CT scanning, microscopy and3D scanning techniques were utilized to characterize the whiskers. Computational fluid dynamics simulations of thewhiskers were carried out to compare them to an ellipse and a cylinder. Leading edge parameters from the whiskerswere used to create a 3D profile based on a modern power turbine blade. The NASA SW-2 facility was used to performwind tunnel cascade testing on the 'Seal Blades'. Computational Fluid Dynamics simulations were used to studyincidence angles from -37 to +10 degrees on the aerodynamic performance of the Seal Blade. The tests and simulationswere conducted at a Reynolds number of 100,000. The Seal Blades showed consistent performance improvements overthe baseline configuration. It was determined that a fuel burn reduction of approximately 5 could be achieved for a fixedwing aircraft. Noise reduction potential is also explored

vortex induced vibration↗

Mars 2020 Rover Adaptive Caching Assembly: Caching Martian Samples for Potential Earth Return

The Adaptive Caching Assembly (ACA) is part of the Sampling and Caching System on the Mars 2020 Perseverance Rover, and consists of multiple stations that process, hermetically seal, and store sample tubes containing collected Martian material, either rock cores or regolith samples, in preparation for caching on the surface of Mars. The ACA stations consist of seven active degrees-of-freedom, as well as a large number of passive mechanisms that must operate in extreme Mars temperature and pressure conditions. A robotic arm within the Rover manipulates the sample tubes between ACA stations as part of an end-to-end sampling sequence, and utilizes a compliant end effector to accommodate misalignments during station interactions. Stringent hardware cleanliness requirements were dictated to ensure collected samples would not be compromised, which significantly impacted the design, assembly, and test operations of the ACA. Three ACAs were assembled to support ground testing and flight operations, which were exposed to environmental testing to validate functionality in Mars-like conditions. A number of challenges existed from design through test, including volume constraints, mechanism controllability and operation, the effects of tight tolerances, and cleanliness requirements.

Lin, Justin↗

Microstructural stability and mechanical properties of the as-cast and heat-treated newly developed TiNbCrTa refractory complex concentrated alloy

In this study, a TiNbCrTa refractory complex concentrated alloy (RCCA) was prepared using vacuum arc remelting. The microstructural evolution and mechanical properties of both as-cast and heat-treated RCCA samples were analyzed. Heat treatment (HT) was performed at 800–1200 °C for 1 h in a vacuum-sealed environment. These samples exhibited a formation of Cr 2 Nb and Cr 2 Ti Laves phases. A variation in elemental distribution was observed, with interdendritic (ID) regions showing higher fractions of Ti and Cr, while the dendritic regions had a greater concentration of Ta and Nb. Micro-segregation at the IDs was confirmed through energy dispersive x-ray spectroscopy mapping, which inferred the formation of Cr- and Ti-rich phases during HT at 800–1200 °C. High-temperature HT at 1200 °C for 1 h led to the evolution of the hcp omega phase. Prolonged HT at 1200 °C for 96 h resulted in the evolution of a Cr-rich Laves phase (Cr 2 Ta), which was homogeneously distributed within the microstructure, indicating an unstable microstructure. Furthermore, despite prolonged HT, a variation in the elemental distribution persisted due to the presence of dendritic and ID regions. Electron backscattered diffraction analysis revealed the presence of bcc and hcp phases in the dendritic and ID regions, respectively, of the as-cast and HTed samples. The as-cast samples demonstrated a high compressive strength of approximately 2 GPa. Micro-hardness values increased with the HT temperature up to 1000 °C. Further increases under HT conditions did not significantly reduce the microhardness value, whereas prolonged HT at 1200 °C led to an increase in the microhardness value. Overall, the newly developed TiNbCrTa RCCA exhibited high-strength behavior even after the phase transformation.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Microgravity ignition experiment

The purpose of this project is to develop a flight ready apparatus of the microgravity ignition experiment for the GASCan 2 program. This involved redesigning, testing, and making final modifications to the existing apparatus. The microgravity ignition experiment is intended to test the effect of microgravity on the time to ignition of a sample of alpha-cellulose paper. An infrared heat lamp is used to heat the paper sample within a sealed canister. The interior of the canister was redesigned to increase stability and minimize conductive heat transfer to the sample. This design was fabricated and tested and a heat transfer model of the paper sample was developed.

Motevalli, Vahid↗

Application of Pinniped Vibrissae to Aeropropulsion

Vibrissae of Phoca Vitulina (Harbor Seal) and Mirounga Angustirostris (Elephant Seal) possess undulations along their length. Harbor Seal Vibrissae were shown to reduce vortex induced vibrations and reduce drag compared to appropriately scaled cylinders and ellipses. Samples of Harbor Seal vibrissae, Elephant Seal vibrissae and California Sea Lion vibrissae were collected from the Marine Mammal Center in California. CT scanning, microscopy and 3D scanning techniques were utilized to characterize the whiskers. Computational fluid dynamics simulations of the whiskers were carried out to compare them to an ellipse and a cylinder. Leading edge parameters from the whiskers were used to create a 3D profile based on a modern power turbine blade. The NASA SW-2 facility was used to perform wind tunnel cascade testing on the 'Seal Blades'. Computational Fluid Dynamics simulations were used to study incidence angles from -37 to +10 degrees on the aerodynamic performance of the Seal Blade. The tests and simulations were conducted at a Reynolds number of 100,000. The Seal Blades showed consistent performance improvements over the baseline configuration. It was determined that a fuel burn reduction of approximately 5 could be achieved for a fixed wing aircraft. Noise reduction potential is also explored.

wakes↗

The Apollo Sample Suite: 50 Years of Solar System Insight

The Apollo program was undoubtable a crowning achievement in human history. In addition to the obvious cultural significance, scientific results from the Apollo program had a lasting impression on a range of scientific fields, none more so that the effect the samples had on the fields of geology and cosmochemistry. The six Apollo missions collected 382 kg of rock, regolith, and core samples from geologically diverse locations on the Moon. In the nearly 50 years since the first samples were returned, there have been over 3000 different requests for samples, each yielding insights into fields as disparate as biology, medicine, astronomy, engineering, material science, and of course geology. Early studies of the Apollo samples revealed primary insights into the origin and evolution of the Moon, and of the Earth-Moon system, but the results also had implications for bodies throughout the solar system, e.g., defining crater counting rates. Over the decades, continued study of the Apollo samples by new generations of scientists using new instruments have continued to yield significant new discoveries, including the presence of endogenous water in the Moon and the possible presence of a lunar cataclysm, that in turn has contributed to new models of solar system formation and evolution. The Apollo samples have often been used as a proxy for studying other bodies like Mercury or asteroids. The Apollo samples have also directly contributed to the interpretation of remotely sensed data sets, including their use as ground truth for both Clementine and Lunar Prospector global geochemical maps. Despite the Apollo samples being a static collection, recent efforts will ensure that investigators continue to have access to new samples. For example, there was a recent solicitation for study of previously unopened Apollo samples in vacuum-sealed containers, as well as new access to samples stored frozen or in a He atmosphere. Similarly, the use of X-ray computed tomography as part of the curation process is identifying new clasts within polymict breccias that are available for study. Finally, the MoonDB project is putting all previously published lunar geochemical analyses into a searchable database, which should facilitate new investigations.

Zeigler, Ryan↗

Volatile/mobile trace elements in meteoritic, non-lunar basalts: Guides to Martian sample contents

A variety of genetic processes on or in extraterrestrial objects can be examined by study of volatile/mobile trace elements. Doubtless, considerable efforts will be expended on determining these elements in returned Martian samples. The purpose is to estimate levels of such elements expected to be present in returned Martian samples. Some ideas about Martian genesis were already advanced from the volatile/mobile element contents in SNC meteorites, assuming that Mars was their parent body. Even is Mars and the SNC meteorite parent body are identical, compositional ranges for returned Martian samples should exceed those of SNC meteorites. It is expected, therefore, that Martian samples returned from locations other than Polar regions will have indigenous volatile/mobile element contents within howardite-diogenite ranges. Elements with strong lithophile tendences may be more abundant, as they are in many lunar samples. Most of these elements should be at ppb levels except for Co, Ga, Zn, and Rb, which should lie at ppm levels. If Martian volcanism was accompanied by fumarolic emanations, it should be reflected in occasional huge enrichments of mobile trance elements, as in lunar meteorite Y 791197. During collection and transport Earthward, samples must be contained under conditions appropriate to ppb concentrations. Materials must be used that will not cause contamination which occurred during the Apollo program, where indium from seals contaminated many samples.

Lipschutz, M. E.↗