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C J Snead

Publications and source records attributed to C J Snead.

Investigating the Effects of Space Weathering in Ryugu Samples Using Coordinated Microanalyses

Airless planetary surfaces are characterized by a distinct lack of an atmosphere or magnetic field, leading to direct exposure to the effects of hypervelocity micrometeoroid impacts and solar wind ion irradiation [1]. These processes, cumulatively known as space weathering, gradually alter the microstructural and chemical properties of the grains on airless surfaces. Signatures of space weathering include vesiculated textures, amorphous grain rims (upper ~100 nm), solar flare tracks, and Fe-bearing nanoparticles (npFe) [2,3]. The accumulation of these microstructural space weathering characteristics, particularly the presence of npFe, alters the spectral properties of airless regoliths resulting in changes in spectral slope and reflectance of the surfaces, and the attenuation of characteristic absorption bands in the visible to near-infrared (Vis-NIR) wavelengths. These spectral changes complicate our ability to accurately interpret the mineralogy of airless bodies via remote sensing spectroscopy [1,4]. Studies of space weathering have primarily focused on anhydrous silicate minerals, reflecting the main components of the available returned samples from the Moon and S-type asteroid Itokawa [3,5,6]. However, our understanding of space weathering of primitive, organic-rich carbonaceous materials is still a work in progress. The Japan Aerospace Exploration Agency (JAXA)’s Hayabusa2 mission offered the first opportunity to directly investigate carbonaceous asteroids by returning samples from C-type asteroid (162173) Ryugu. Initial studies of Ryugu samples show mineralogical similarities to CI chondrites along with surface modifications consistent with space weathering. These surface modifications are primarily in the form of μm-thick silicate melts, amorphized phyllosilicates, glassy spherules, and burst vesicles [3,7]. Here, we report results from coordinated microanalytical techniques to further our understanding of the mineralogy and space weathering of carbonaceous materials.

L E Melendez

An Improved Hf Vapor Etching Apparatus for Stardust Particle Extraction

Introduction: The NASA Stardust mission captured thousands of particles from the Jupiter-family comet 81P/Wild 2 in a collector composed of aluminum foil and blocks of silica aerogel [1]. To date, most Wild 2 particles available for study are relatively large and coherent particles extracted individually from the ends of hollow, carrot-shaped impact tracks produced during impact into aerogel. However, >65% of the impacting mass can be found in the ‘bulb’ of the track, including nearly all of the <1 μm size fraction [2]. This fraction contains organic-rich material and is likely to include presolar grains, representing a critical opportunity to constrain the organic and presolar inventory of primitive outer solar system materials. However, the small size and susceptibility of this fraction to melting or alteration during capture poses significant analytical challenges. Previous attempts to extract and concentrate fine-grained material from the bulb of Stardust tracks have attempted to develop techniques that efficiently destroy aerogel and leave impactor particles relatively unharmed. The low density and high porosity of silica aerogel makes it more susceptible to attack by etching with hydrofluoric acid (HF) [3] or CF4 plasma ashing [4] than collected cometary silicates. Previous studies of HF vapor etching used HF solutions varying between 5 to 49% and noted that at high concentrations and etch rates, a liquid droplet was produced according to the etching reaction 4HF + SiO2 → SiF4 (g) + 2H2O [3]. SiF4 readily decomposes into HF and silicic acid in water, which has the potential to alter the freed cometary silicates. The plasma ashing technique avoids production of a liquid droplet and minimizes damage to embedded silicates but requires specialized equipment [4]. In this abstract, we present recent improvements to the HF etching procedure with the aim of constructing an etching chamber capable of slowly etching silica aerogel using small quantities of dilute HF. The etching chamber can be assembled using readily available materials.

Stardust

Microbial Monitoring of New Cleanrooms Used to Curate Astrobiologically Relevant Asteroid Samples from Bennu and Ryugu

Introduction: NASA has constructed two new cleanrooms to house materials from the OSRIS-REx and Hayabusa2 missions to the asteroids Ryugu (162173) and Bennu (101955), respectively. In accordance with standard astromaterials curation practices, these cleanrooms will be monitored for particulate contamination and maintained to ISO 5 equivalent standards1. Since the samples in these collections are expected to contain prebiotic organic compounds that may help explain the origin of life on Earth, these labs will also be monitored for organic and biological contamination2. Samples from Ryugu arrived on Earth in December, 2020. After basic characterization in Japan, NASA received a subset of these samples at the astromaterials curation facility in Houston in December of 2021. OSIRIS-REx is expected to return samples in September, 2023. Here we present preliminary microbial monitoring results from monthly monitoring of these new labs and the connected microtomy and staging areas that support them, as they are being commissioned. We also compare these results to baseline values for other astromaterials curation labs. We will also briefly describe additional cleaning efforts employed to reduce the bioburden in these new cleanrooms. Methods: Microbial samples were collected from surfaces using a dry macrofoam swab (Puritan Brand 2518051PFRNDFD). Swabs were also opened in the lab but not touched to any surfaces to function as negative controls. Samples and controls were processed inside a class II biosafety cabinet to avoid inadvertent cross contamination. The swabs were suspended in 15 ml of PBS (Phosphate Buffered Saline) and vortexed for 20 seconds to remove cells from the swab surface. The PBS was used to inoculate Petri dishes filled with TSA (Tryptic Soy Agar), Blood Agar, or Reasoners 2 agar to check for microbial growth. Each plate was inoculated with 0.1 ml of PBS. The TSA and blood agar plates were incubated at 35˚C and the Reasoners 2 agar plates were incubated at 25˚C for seven days. Petri dishes filled with Potato dextrose agar, Saboraud dextrose agar, or Saboraud dextrose agar with 0.1 mg/ml of chloramphenicol, an antibiotic, were used to check for fungal growth. These plates were inoculated with 0.3 ml of PBS and incubated at 30˚C. The remaining PBS was frozen at -80 ˚C for DNA sequencing. After incubation, isolates were counted and reisolated for identification. Isolates were identified using the VITEK23 system or by sequencing a portion of the 16S rRNA gene for bacteria or the ribosomal internal transcribed spacer (ITS) for fungi. Sequencing was performed with an ABI 3500 Sanger sequencer. Results: During our initial sampling, six of the seven sites sampled (86%) displayed bacterial or fungal growth. Samples collected from the staging areas and microtomy labs are not included in this calculation since those areas are maintained at a lower ISO 7 equivalent cleanliness standard. A month later, only three of the seven sites (43%) displayed bacterial growth. No fungal growth was detected in the second sampling. Since new equipment had been introduced to the Hayabusa2 lab since the first round of sampling, an additional three sampling sites were included in the second round of sampling. None of these sites displayed microbial growth. These sites will be included in all future sampling efforts. Bacterial isolates have been identified from the following genera at multiple time points: Micrococcus, Staphylococcus, and Bacillus. Isolates from the genera: Microbacterium, Nocardioides, Methylocystis, and Microvirga were identified in the initial sampling, but were not present at later time points. Identification of fungal isolates is in progress. Results are summarized in Table 1. Discussion: The recovery rate or percentage of positive samples4 was initially 86%, which is higher than the median recovery rate for comparable ISO 5 equivalent curation labs like Stardust (33%), Hayabusa (33%), and Cosmic Dust (50%). However, after a month of operation, the recovery rate for these same sites decreased to 43%, which is similar to what we observe in comparable curation cleanrooms with no microbial control requirements. Adding in the new sampling sites further decreases the recovery rate to 30%. With the reduction in recovery rate, we also observed a decrease in microbial diversity. At the first time point, we observed at least 10 different bacterial species and at least two different fungi. This is a higher diversity than the median values for comparable ISO 5 equivalent labs (2-4 isolates per sampling event). After the second sampling, we observed at least 4 bacterial species and no fungi, which is more consistent with comparable labs. We expect the recovery rate and diversity in both labs to continue to decrease as routine operation continues. We will use ultrapure hydrogen peroxide to disinfect equipment and work areas prior to opening any sample containers. Most of the bacterial and fungal isolates were detected on samples from the cleanroom floors. This is consistent with baseline results from other curation labs. Organisms from the genera Bacillus, Staphylococcus, and Micrococcus that were repeatedly detected are common in cleanrooms and on human skin5,6. These organisms are generally thought to be introduced when people enter the cleanroom. Microbacterium, Nocardioides, and Microvirga have also previously been identified in astromaterials cleanrooms, but not as frequently as Bacillus, Staphylococcus, and Micrococcus. Methylocystis is a novel genus in the astromaterials cleanrooms, but it was identified with low accuracy (93% match in the sequenced region of the 16S rRNA gene) and further work is needed to confirm this identification. Microbacterium is a diverse genus with isolates identified from terrestrial and aquatic sediments. Some species of Microbacterium are capable of degrading complex organic compounds found in crude oil. The presence of these bacteria in the OSIRIS REx and Hayabusa2 cleanrooms should be closely monitored. Methylocystis is a genus of methanotrophic bacteria capable of oxidizing methane. If this identification proves to be correct and it is detected again, it should be closely monitored as well. Under nominal operating conditions, samples should not ever encounter the cleanroom floor or other high traffic areas. If we observe an increase in the bioburden in sensitive work areas that appears to be influenced by organism transfer from high traffic areas like the floors, we can employ additional hydrogen peroxide treatments to disinfect high traffic areas. Routine microbial monitoring of these labs will ensure that NASA’s astromaterials collections remain pristine and useful for scientific study. Table 1. Sampling Locations and Colony Counts Bacterial CFUa Fungal CFU Bacterial CFU Fungal CFU Lab - Location 11/2/2021 11/2/2021 12/13/2021 12/13/2021 H2b-Floor 4 8 1 0 H2-staging pass through 3 0 0 0 H2-microtomy pass through TNTCc 0 0 0 H2 Microscope 1 NA NA 0 0 H2 Microscope 2 NA NA 0 0 H2-Table NA NA 0 0 OREXd- microtomy pass through 0 0 6 0 OREX – Anteroom pass through 0 0 0 0 OREX – Floor 1 2 0 0 OREX Witness Foil Table 3 0 1 0 Staging-Floor 16 0 15 0 Microtomy-Floor 3 0 2 0 a: CFU = Colony Forming Unit b: H2 = Hayabusa2 Lab c: TNTC = too numerous to count d: OREX = OSIRIS-REx Lab References: 1. ISO 14644-1:2015 - Cleanrooms and associated controlled environments -- Part 1: Classification of air cleanliness by particle concentration. 37 (2015). 2. McCubbin, F. M. et al. Space Sci Rev 215, (2019). 3. Pincus, D. H. Encyclopedia of Rapid Microbiological Methods (2005). 4. The United States Pharmacopeial Convention. USP General Chapter <1116> 17, 784–794 (2013). 5. Sheraba, N. S., Yassin, A. S. & Amin, M. BMC Research Notes 3, 278 (2010). 6. Utescher, C. L. de A., Franzolin, M. R., Trabulsi, L. R. & Gambale, V. Brazilian Journal of Microbiology 38, 710–716 (2007).

A B Regberg

EVALUATION OF OSIRIS-REx CONTACT PAD SAMPLERS FOR BENNU SURFACE REGOLITH PARTICLES.

NASA’s Origins, Spectral Interpretation, Resource Identification, and Security–Regolith Explorer (OSIRIS-REx) mission returned material from asteroid Bennu to Earth in September 2023. In addition to the bulk sample (>70 g), OSIRIS-REx’s Touch-and-Go Sample Acquisition Mechanism (TAGSAM) also collected material from Bennu using surface particle collectors or contact pads. The TAGSAM head has 24 of these circular contact pads evenly distributed around the perimeter, each ~1.75 cm in diameter and consisting of stainless-steel Velcro-like loops. From their positions on the bottom of the TAGSAM head, the contact pads were intended to collect regolith material from the very surface of Bennu by trapping fine particles (<5 mm) in the Velcro. The science team would then be able to examine individual particles for evidence of surface exposure, particularly the microstructural, chemical, and spectral characteristics of space weathering. Here we present an evaluation of the OSIRIS-REx contact pads and the material they returned from Bennu.

M. S. Thompson

Assessing the Oxygen Permeability of Candidate Asteroid Sample Containers With Optochemical Sensors

The Astromaterials Acquisition and Curation Office at NASA Johnson Space Center currently curates 500 mg (10%) of carbonaceous asteroid Ryugu regolith collected by the Japan Aerospace and Exploration Agency’s Hayabusa II spacecraft and returned to Earth in 2021. In September 2023, NASA’s OSIRIS-REx spacecraft returned at least 70 grams of regolith collected from the surface of Carbonaceous Asteroid Bennu. These new astromaterials collections are stored and handled in gloveboxes and desiccators that are continuously purged with ultrapure nitrogen in order to minimize contamination and alteration of extraterrestrial samples from terrestrial environments, e.g., reaction with terrestrial oxygen and water. Ito et al. have previously reported on the development of containers to transport samples between facilities in inert, sealed environments; Hayabusa2 samples allocated to investigators by JAXA’s Extraterrestrial Sample Curation Center (ESCuC) are shipped in these Facility-to-Facility Transfer Containers (FFTCs). NASA curation has also been investigating sealed containers for storage, transportation, and allocation of Bennu and Ryugu regolith in sealed anoxic environments. In order to assess the ability of candidate sample containers to maintain nitrogen environments, we have utilized optochemical sensors to measure trace oxygen levels within sealed volumes.

C J Snead

Trace Oxygen Measurements of Asteroid Sample Storage Desiccators

The Astromaterials Curation facility at the NASA Johnson Space Center is currently curating more than 120 g of carbonaceous asteroid Bennu material as well as over 500 mg of asteroid Ryugu [1 and 2]. These astromaterials are stored in isolating desiccators and gloveboxes under a continuous purge of pure (<1 ppm O 2 ) gaseous nitrogen. The oxygen and moisture concentrations in our OSIRIS-REx sample processing gloveboxes are continuously monitored via integrated sensors; however, our sample storage desiccators lack integrated oxygen and humidity sensors. In previous studies, we used PreSens Fibox 4 trace oxygen meters and optochemical PSt9 spot sensors to measure the oxygen concentrations in candidate asteroid sample containers that had been sealed in nitrogen; we determined that Eagle stainless steel containers inhibit the ingress of external oxygen for several weeks [3]. This optochemical sensor technology allowed us to take precise, contactless measurements within a trace range of 0 to 200 ppmv O 2 . The effectiveness of the trace oxygen sensors in our container experiments inspired us to utilize them to assess the performance of our desiccators that previously lacked trace oxygen monitoring. In this study, our goal was to determine the quality of the nitrogen purge in the isolating desiccator under normal operating conditions by measuring the trace oxygen content. Utilizing optochemical sensor technology, we determined how long the oxygen concentration takes to reach an equilibrium in the desiccator; that is, determine the rate at which the oxygen diffusion into the desiccator equals the rate at which oxygen diffuses out of the desiccator via N2 purge. Additionally, we wanted to determine the oxygen concentration at this equilibrium, the state in which our desiccators are in during normal operating conditions. We tested a custom three chamber desiccator manufactured by Germfree using a PSt9 trace oxygen sensor spot that was mounted into a ¼” National Pipe Tapered (NPT) metal flow-through cell and attached it to the desiccator exhaust. The desiccator consists of top, middle, and bottom isolating chambers. The top chamber door was opened for several minutes to simulate a sample exchange, it was sealed, and then purged ~15 Standard Cubic Feet per Hour (SCFH). Oxygen measurements were automatically recorded via the Fibox 4 trace oxygen meter in 5-minute intervals over the course of a 24-hour period. Our results indicate the desiccator reached an equilibrium value of 10-15 ppm O 2 after ~5 hours (Fig. 1). This data allows us to explore standards for purging and exchange protocols that can be applied to similar types of desiccators in Hayabusa2, OSIRIS-REx, and for sample return collections. The assessment of the internal gaseous compositions of desiccators also allows us to share with the community the N 2 environment in which many of our asteroid samples and hardware are securely curated. Future measurements will include other nitrogen flow rates and measuring the trace oxygen concentration as a function of time for the levels of the previous commercial desiccator in which the Hayabusa2 sample collection was stored. We will also analyze how long the desiccators hold N2 after being disconnected from their N2 source, an extended measurement for sample security reassurance.

Curation