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NASA NTRS2008

Miniature Mass Spectrometers on Space and Planetary Missions

Space flight mass spectrometers contribute our understanding of the origin and evolution of our solar system and even of life itself. This fundamental role has motivated increasing interest in miniature mass spectrometry for planetary missions. Several remarkable new instruments are en route or under development to investigate the composition of planetary bodies such as Mars and comets. For instance, the Sample Analysis at Mars (SAM) suite on the 2009 Mars Science Laboratory (MSL) mission includes a quadrupole mass spectrometer with a sophisticated gas processing system as well as pyrolysis and chemical derivatization protocols for solid samples. Future missions will require even lighter, lower power, and yet more capable mass spectrometers, particularly to analyze samples in situ on planetary surfaces. We have been developing laser-based mass spectrometers for elemental and organic/molecular analysis of rock, ice, or fine particle samples. These typically use time-of-flight (TOF) mass analyzers, which are readily miniaturized and can detect both atomic species and complex organics that occur in a variety of planetary materials. For example, nonvolatile polycyclic aromatic hydrocarbons and kerogen-like macromolecular carbon are found in some carbonaceous meteorites, which derived from asteroid parent bodies. A single focused laser pulse is able to volatilize and ionize some of these compounds for direct TOF analysis. While this is possible without any sample preparation or contact, sensitivity and quantitative performance can improve significantly with some sample handling. As such we have also been examining robotic mechanisms and protocols to accompany space flight mass spectrometers. In addition, sensors in early development may significantly improve these capabilities, via use of techniques such as switchable polarity, ambient pressure, or resonant ionization; tandem mass spectrometry (TOF or ion trap); and chemical imaging.

Brinckerhoff, William↗
NASA NTRS1983

Profiles and intensity ratios of the C IV lambda 1548, 1550 emission lines in planetary nebulae

The C IV resonance doublet at lambda 1548, 1550 is an important diagnostic tool in the study of planetary nebulae. The predicted theoretical intensity ratio of 2:1 is, however, rarely observed in the high dispersion IUE spectrograms. Values of 0.8-2.0 are observed for a sampling of 11 planetary nebulae of various excitation classes and for three proto-planetary nebulae. A diversity of line profiles is observed. In addition to the C IV doublet, weak subsidiary lines are seen. The spacing between these pseudo-lines happens to correspond to the separation of the C IV lines but are believed to be due to hot pixels and do not conform to the radial velocity displacement of the C IV lines.

Feibelman, W. A.↗
NASA NTRS2022

Development Towards Stable Chlorine Isotope Measurements of Astromaterials Using the Modified Middleton Source of an Accelerator Mass Spectrometer

The volatile element Cl can be lost during the formation and evolution of planetary bodies, leading to fractionation of its two stable isotopes 35Cl and 37Cl. Chlorine isotope variations (reported as δ37Cl in parts per thousand (‰) relative to Standard Mean Ocean Chloride, SMOC) are documented to exceed 80‰ between different lunar rock samples and have been variably interpreted as the fingerprint of degassing during accretion, magma ocean, or volcanic portions of lunar history. The large intersample and intrasample variations observed by both bulk isotope ratio mass spectrometry (IRMS) and in-situ secondary ion mass spectrometry (SIMS) methods are difficult to interpret in part because of a paucity of bulk Cl isotope measurements. This lack of high-precision bulk data is due to the relative rarity of IRMS laboratories capable of making these high precision measurements on small samples of precious planetary materials such as those returned by human or robotic exploration. Here we present a new method for performing high precision δ37Cl measurements using the modified Middleton ion source of an existing accelerator mass spectrometer. For samples with as little as 1 μg Cl–the equivalent of 2–4 mm3 of a typical lunar rock sample–the average cathode accuracy is ∼1‰. Cathode reproducibility is typically ∼1‰ (2σ) for samples with at least 10 μg of Cl, increasing to ∼3–6‰ for aliquots with ∼1–2 μg Cl, similar to published SIMS results and sufficient to study astromaterials from the Moon, Mars, or 4 Vesta, which have tens of ‰ observed variations.

Tyler S. Anderson↗
NASA NTRS2017

Mobile/Modular BSL-4 Facilities for Meeting Restricted Earth Return Containment Requirements

NASA robotic sample return missions designated Category V Restricted Earth Return by the NASA Planetary Protection Office require sample containment and biohazard testing in a receiving laboratory as directed by NASA Procedural Requirement (NPR) 8020.12D - ensuring the preservation and protection of Earth and the sample. Currently, NPR 8020.12D classifies Restricted Earth Return for robotic sample return missions from Mars, Europa, and Enceladus with the caveat that future proposed mission locations could be added or restrictions lifted on a case by case basis as scientific knowledge and understanding of biohazards progresses. Since the 1960s, sample containment from an unknown extraterrestrial biohazard have been related to the highest containment standards and protocols known to modern science. Today, Biosafety Level (BSL) 4 standards and protocols are used to study the most dangerous high-risk diseases and unknown biological agents on Earth. Over 30 BSL-4 facilities have been constructed worldwide with 12 residing in the United States; of theses, 8 are operational. In the last two decades, these brick and mortar facilities have cost in the hundreds of millions of dollars dependent on the facility requirements and size. Previous mission concept studies for constructing a NASA sample receiving facility with an integrated BSL-4 quarantine and biohazard testing facility have also been estimated in the hundreds of millions of dollars. As an alternative option, we have recently conducted an initial trade study for constructing a mobile and/or modular sample containment laboratory that would meet all BSL-4 and planetary protection standards and protocols at a faction of the cost. Mobile and modular BSL-2 and 3 facilities have been successfully constructed and deployed world-wide for government testing of pathogens and pharmaceutical production. Our study showed that a modular BSL-4 construction could result in approximately 90% cost reduction when compared to traditional construction methods without compromising the preservation of the sample or Earth.

Calaway, M. J.↗
NASA NTRS2005

Atmospheric Electron-induced X-Ray Spectrometer (AEXS) Instrument Development

Introduction: This paper describes the progress in data acquisition and establishing the observational capability of the AEXS instrument. The AEXS is a miniature instrument[1-4] based on the excitation of characteristic X-Ray Fluorescence (XRF) and luminescence spectra using a focused electron beam which enables nondestructive evaluation of sample surfaces in planetary ambient atmospheres. In situ operation is obtained through the use of a thin electron transmissive membrane to isolate the vacuum of the AEXS source from the outside ambient atmosphere. Thus eliminating the need for a vacuum pumped sample chamber as is common in all laboratory SEM s. The transmitted electrons impinge on the sample exciting XRF spectra from the irradiated spot on in-situ or collected samples with sub-mm to cm-scale spatial resolution at Mars atmospheric pressure. The AEXS system (Fig 1) consists of a high-energy (>10keV) electron gun encapsulated by the isolation membrane, an XRF detection and analyzer system, and a high voltage power supply. The XRF data are analyzed to determine the elemental abundance for the irradiated spots. The approach to demonstrating a proof of concept of the AEXS has been through 1) demonstrating the viability of microfabricated membranes, 2) assembling AEXS setups with increasingly integrated functional components, and 3) simulating the AEXS observational capabilities. The development of the instrument is described in detail in the poster paper[4] at this conference. This paper focuses on describing the progress of the AEXS instrument to acquire XRF data and using commercially available software to analyze the data streams and determine the accuracy, precision and resolution of the analysis compared to the certified elemental abundance.

Urgiles, E.↗
NASA NTRSDate not supplied

Stable Chlorine Isotope Measurements of Astromaterials Using the Cs-Sputter Negative Ion Source of an Accelerator Mass Spectrometer

The volatile element Cl can be lost during the formation and evolution of planetary bodies, leading to fractionation of its two stable isotopes 35Cl and 37Cl. Chlorine isotope variations (reported as δ37Cl in parts per thousand (‰) relative to Standard Mean Ocean Chloride, SMOC) [1] are documented to exceed 80‰ [2] between different lunar rock samples and have been variably interpreted as the fingerprint of degassing during accretion, magma ocean, or volcanic portions of lunar history[3,4].The large intersample and intrasample variations observed by both bulk isotope ratio mass spectrometry (IRMS) and in-situ secondary ion mass spectrometry (SIMS) methods are difficult to interpret in part because of a paucity of bulk Cl isotope measurements (Figure 1).This lack of high-precision bulk data is due to the relative rarity of IRMS laboratories capable of making these high precision measurements on small samples of precious planetary materials such as those returned by human or robotic exploration. Here we present a new method for performing high precision δ37Cl measurements using the Cs-sputter negative ion source of an existing accelerator mass spectrometer. A brief description of the methods used for this work is followed by the results of our δ37Cl measurements and a discussion of the technique’s possible applications.

Chlorine↗
NASA NTRS1997

Planetary and Primitive Object Strength Measurements and Sampling Apparatus

We present experimental data and a model for the low-velocity (subsonic, 0 - 1000 m/s) penetration of brittle materials by both solid and hollow (i.e., coring) penetrators. The experiments show that penetration is proportional to momentum/frontal area of the penetrator. Because of the buildup of a cap in front of blunt penetrators, the presence or absence of a streamlined or sharp front end usually has a negligible effect for impact into targets with strength. The model accurately predicts the dependence of penetration depth on the various parameters of the target-penetrator system, as well as the qualitative condition of the target material ingested by a corer. In particular, penetration depth is approximately inversely proportional to the static bearing strength of the target. The bulk density of the target material has only a small effect on penetration, whereas friction can be significant, especially at higher impact velocities, for consolidated materials. This trend is reversed for impacts into unconsolidated materials. The present results suggest that the depth of penetration is a good measure of the strength, but not the density, of a consolidated target. Both experiments and model results show that, if passage through the mouth of a coring penetrator requires initially porous target material to be compressed to less than 26% porosity, the sample collected by the corer will be highly fragmented. If the final porosity remains above 26%, then most materials, except cohesionless materials, such as dry sand, will be collected as a compressed slug of material.

Ahrens, Thomas J.↗
NASA NTRS2016

Modeling of Active Tether System Concepts for Planetary Exploration

This paper summarizes an approach for modeling, simulation, and control of tethered systems in which the tether is actively controlled. Various aspects of the system model are described, including tether dynamics, end-effector dynamics, contact interaction and the model of the active tether material. We consider three scenarios: a tether made of an electrically switchable material for small body sampling, a tether for close-proximity operations such as capture and grappling, and a tether harpooning to a small body for sample capture or planetary fly-by.

Quadrelli, Marco B.↗
NASA NTRS2003

New Methods of Sample Preparation for Atom Probe Specimens

Magnetite is a common conductive mineral found on Earth and Mars. Disk-shaped precipitates approximately 40 nm in diameter have been shown to have manganese and aluminum concentrations. Atom-probe field-ion microscopy (APFIM) is the only technique that can potentially quantify the composition of these precipitates. APFIM will be used to characterize geological and planetary materials, analyze samples of interest for geomicrobiology; and, for the metrology of nanoscale instrumentation. Prior to APFIM sample preparation was conducted by electropolishing, the method of sharp shards (MSS), or Bosch process (deep reactive ion etching) with focused ion beam (FIB) milling as a final step. However, new methods are required for difficult samples. Many materials are not easily fabricated using electropolishing, MSS, or the Bosch process, FIB milling is slow and expensive, and wet chemistry and the reactive ion etching are typically limited to Si and other semiconductors. APFIM sample preparation using the dicing saw is commonly used to section semiconductor wafers into individual devices following manufacture. The dicing saw is a time-effective method for preparing high aspect ratio posts of poorly conducting materials. Femtosecond laser micromachining is also suitable for preparation of posts. FIB time required is reduced by about a factor of 10 and multi-tip specimens can easily be fabricated using the dicing saw.

rock varnish↗
NASA NTRS2003

In-Space Propulsion: Where We Stand and What's Next

The focus of this paper will be on the three stages of in-space transportation propulsion systems, now commonly referred to as in-space propulsion (ISP); i.e., the transfer of payloads from low-Earth orbits into higher orbits or into trajectories for planetary encounters, including planetary landers and sample return launchers, if required. Functions required at the operational location where ISP must provide thrust for orbit include maintenance, position control, stationkeeping, and spacecraft altitude control; i.e., proper pointing and dynamic stability in inertial space; and the third function set to enable operations at various planetary locations, such as atmospheric entry and capture, descent to the surface and ascent, back to rendezvous orbit. The discussion will concentrate on where ISP stands today and some observations of what might be next in line for new ISP technologies and systems for near-term and future flight applications. The architectural choices that are applicable for ISP will also be described and discussed in detail.

Sackheim, Robert L.↗
NASA NTRSDate not supplied

AERACEPT (Aerosol Rapid Analysis Combined Entry Probe/sonde Technology): Enabling Technology for Planetary Atmospheric Science Probes

Aerosols –clouds, hazes, and dusts –are a key part of planetary mass and energy balance, but difficult to study remotely. Current technology limits in situ measurements to once-in-a-lifetime flagship missions, which is not enough to characterize such highly dynamic systems. AERACEPT (AErosol Rapid Analysis Combined Entry Probe/sonde Technology) is an early-stage technology allowing asingle aeroshell body toact as both anentry vehicle and aerosol-samplingpassivedescent sonde, using the aeroshell’sown velocityto drive aerosol capture and separationthrough a series of embedded inlets.It takes advantage ofrecently developed thermal protection materials (3D-CC and 3MDCP)in combination withheritage aerosol sampling technologies fromboth planetary and airborne science (high-speed inlets and particle separation). By eliminating the need for heat shield separation, deployable parachutes, ordescent control, AERACEPT reducesthe mass, volume, and complexity ofplanetary aerosol sampling. Verifying AERACEPT’s performance involves modeling interdependencies between the size and geometry of the sampling inlets, the material response of the hypersonic phase of entry, the thermal conditions throughout the probe’s descent, the subsonic flow and particle sampling efficiency, the needed amount of sample, andthe cadence at which the sample can be analyzed. AERACEPT’s current predictions, using the Nephele Venus cloud mission concept (sampling between 63km to 39km, all subsonic) indicates AERACEPT can obtain >20 μL of particle material (roughly 10x the limit of detection) from droplets larger than 0.2 μm, with sample heating limited to <15 K above ambient. Validation testing for the thermal material response model has recently been performed at the UIUC Plasmatron facility, and for the flow and particle capture models is planned for this fall at the Ames Fluid Mechanics Laboratory.

AERACEPT↗
NASA NTRS2019

Introducing NASA Ames' New Infrared Optical Constant Facility. Determinations of Complex Refractive Indices for Titan Aerosol Analogs and Other Applications

A new optical constant facility has been developed at NASA Ames that will allow the determination of optical constants in the infrared of various materials, analogs of (exo)planetary hazes and cloud particles. Our facility is composed of a Fourier Transform Infrared (FTIR) spectrometer continuously covering the Near-IR to Far-IR range (from 0.74 to 200 μm), coupled to variable angle transmittance and reflectance accessories that allow the characterization of the scattering properties of non-homogeneous samples (laboratory (exo)planetary aerosol analogs, films, slabs of material, crystals, powders, etc.) over a wide incidence and emittance angle range (0-90 degrees). This new experimental setup allows the characterization of angular light distribution in both transmission and reflection measurements, and enables the determination of the complex indices of refraction, n and k, over the full NIR-FIR range via modeling of the laboratory measurements. The resulting refractive indices are critical input parameters in radiative transfer models, microphysical models, cloud models, protoplanetary disk simulations and other models used for the interpretation of observational data from past, current and future (exo)planetary NASA missions. Here we present a description of the facility along with the first determination of optical constants for Titan aerosol analogs produced in the Titan Haze Simulation (THS) experiment on COSmIC, a unique experimental setup developed at NASA Ames that allows the simulation of Titan’s complex atmospheric chemistry at Titan-like temperature (200 K). We also introduce a new study of the optical properties of ammonium-bearing phosphates, potential cloud particles forming in temperate exoplanets and brown dwarfs.

Sciamma-O'Brien, Ella M.↗
NASA NTRS1972

Detection of metabolically produced labeled gas - The Viking Mars Lander.

A qualitative, nonspecific method will test for life on Mars in 1976 by supplying radioactive substrates to samples of the planetary surface material. If microorganisms are present, they may assimilate one or more of the simple labeled compounds and produce radioactive gas. The compounds have been selected on the basis of biological theory and terrestrial results. The measurement of radioactive gas evolved as a function of time constitutes evidence for life. A control performed on a duplicate, but heat sterilized, sample will confirm the biological nature of the results. The shape of the response curve obtained from the viable sample may provide information on the physiological state and generation period of the organisms. Data obtained from a wide variety of terrestrial soils demonstrate a rapid response and high sensitivity for the experiment. Its ability to make comparative studies of soil microorganisms is also demonstrated.

Levin, G. V.↗
NASA NTRSDate not supplied

From Apollo to Artemis: How Processing ANGSA Core Samples 73001/2 Can Help to Prepare for Future Sample Return Missions to the Moon and Beyond.

Introduction: Apollo Sample 73001/2 is a ~71cm long double drive tube consisting of an upper part (73002) and a lower part (73001) that contains regolith collected near Lara Crater at the Apollo 17 site, Station 3. The double drive tube is believed to have penetrated a lunar landslide deposit that was transported from the slope of the South Massif into the Taurus-Littrow Valley [1]. As part of the ANGSA (Apollo Next Generation Sample Analyses) initiative, preparing a preliminary examination (PE) catalog of 73001/2 is a crucial first step for the early identification of material types such as rock fragments and potential stratigraphy within the core. Many new curation and scientific tools such as X-ray computed tomography (XCT) [3], multi-spectral imaging [4], and gas extraction manifold with piercing tool [5-7], have been applied to the ANGSA core to benefit curation strategy, PE efforts, sample allocation to the planetary science community, and ultimately help to prepare for future sample return missions like Artemis. 73001/2 Preliminary Examination and Processing: Sample 73002 was successfully opened and extruded in Nov. 2019 and fully dissected at the end of 2021. Sample 73001 (Fig. 1) was successfully extruded in March 2022 after careful planning before opening the Core Sample Vacuum Container (CSVC) that was holding the drive tube of 73001. XCT, as part of PE, was used to scan the bottom and top part of the 73001 core tube within the CSVC prior to opening it to 1) facilitate non-destructive, rapid detection of any contamination potentials due to piercing of the CSVC during gas extraction [7]; and 2) to aid in the Artemis sample tool development and provide data on the knife edge seal of the CSVC. This knowledge will help us connect the mechanics of the implemented design (i.e., XCT data) to the performance of the seal (i.e., data on the gas samples will tell us how well the seal preserved the volatile record of lunar samples). Both type of information will feed forward into Artemis tool and storage strategies for future samples. Results and Lessons learned: The XCT data of the CSVC and core tube within showed that the bottom Teflon cap was not pierced during gas extraction (Fig. 1c) and thus, the sample integrity remained guaranteed during piercing and subsequent gas extraction. However, the XCT scan of the top of the core (Fig. 1b) revealed that the drive tube was overfilled with lunar soil and the tool that keeps the soil constrained within the drive tube was not fully deployed. These preliminary data allowed us to implement the necessary steps to prevent loss of sample integrity, including any potential stratigraphy shifts during extrusion. Processing Apollo core 73001/2, creating an informative PE catalog, and applying new and refined tools and technologies for sample analyses are invaluable activities that will assist in circumventing any potential pitfalls, aid in the characterization of samples, and help in the assessment of how well any lunar material has been collected and preserved in the past. This will aid in designing future sample collections and curation procedures and help to prepare for future human exploration and sampling missions such as Artemis. References: [1] Schmitt H. (2017) Icarus 298, 2-33. [3] Zeigler et al. (2021) LPSC 52nd, #2632; [4] Sun et al. (2021), LPSC 52nd, #1789; [5] Parai et al. (2021), LPSC 52nd #2665; [6] Schild et al. (2021) LPSC 52nd #1888; [7] McDonald (2022) ESL 2022.

ANGSA↗
NASA NTRS1991

A perception and manipulation system for collecting rock samples

An important part of a planetary exploration mission is to collect and analyze surface samples. As part of the Carnegie Mellon University Ambler Project, researchers are investigating techniques for collecting samples using a robot arm and a range sensor. The aim of this work is to make the sample collection operation fully autonomous. Described here are the components of the experimental system, including a perception module that extracts objects of interest from range images and produces models of their shapes, and a manipulation module that enables the system to pick up the objects identified by the perception module. The system was tested on a small testbed using natural terrain.

Choi, T.↗
NASA NTRS2001

Mars Sample Handling Protocol Workshop Series: Workshop 2a (Sterilization)

The Space Studies Board of the National Research Council provided a series of recommendations to NASA on planetary protection requirements for future Mars sample return missions. One of the Board's key findings suggested, although current evidence of the martian surface suggests that life as we know it would not tolerate the planet's harsh environment, there remain 'plausible scenarios for extant microbial life on Mars.' Based on this conclusion, all samples returned from Mars should be considered potentially hazardous until it has been demonstrated that they are not. In response to the National Research Council's findings and recommendations, NASA has undertaken a series of workshops to address issues regarding NASA's proposed sample return missions. Work was previously undertaken at the Mars Sample Handling and Protocol Workshop 1 (March 2000) to formulate recommendations on effective methods for life detection and/or biohazard testing on returned samples. The NASA Planetary Protection Officer convened the Mars Sample Sterilization Workshop, the third in the Mars Sample Handling Protocol Workshop Series, on November 28-30, 2000 at the Holiday Inn Rosslyn Westpark, Arlington, Virginia. Because of the short timeframe between this Workshop and the second Workshop in the Series, which was convened in October 2000 in Bethesda, Maryland, they were developed in parallel, so the Sterilization Workshop and its report have therefore been designated as '2a'). The focus of Workshop 2a was to make recommendations for effective sterilization procedures for all phases of Mars sample return missions, and to answer the question of whether we can sterilize samples in such a way that the geological characteristics of the samples are not significantly altered.

Rummel, John D.↗