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All sourcesNASA NTRSDOE OSTI
NASA NTRS2012

In Situ Geochemical Analysis and Age Dating of Rocks Using Laser Ablation-Miniature Mass Spectrometer

A miniaturized instrument for performing chemical and isotopic analysis of rocks has been developed. The rock sample is ablated by a laser and the neutral species produced are analyzed using the JPL-invented miniature mass spectrometer. The direct sampling of neutral ablated material and the simultaneous measurement of all the elemental and isotopic species are the novelties of this method. In this laser ablation-miniature mass spectrometer (LA-MMS) method, the ablated neutral atoms are led into the electron impact ionization source of the MMS, where they are ionized by a 70-eV electron beam. This results in a secondary ion pulse typically 10-100 microsecond wide, compared to the original 5-10-nanosecond laser pulse duration. Ions of different masses are then spatially dispersed along the focal plane of the magnetic sector of the miniature mass spectrometer and measured in parallel by a modified CCD (charge-coupled device) array detector capable of detecting ions directly. Compared to conventional scanning techniques, simultaneous measurement of the ion pulse along the focal plane effectively offers a 100% duty cycle over a wide mass range. LAMMS offers a more quantitative assessment of elemental composition than techniques that detect laser-ionized species produced directly in the ablation process because the latter can be strongly influenced by matrix effects that vary with the structure and geometry of the surface, the laser beam, and the ionization energies of the elements. The measurement of high-precision isotopic ratios and elemental composition of different rock minerals by LAMMS method has been demonstrated. The LA-MMS can be applied for the absolute age determination of rocks. There is no such instrument available presently in a miniaturized version that can be used for NASA space missions. Work is in progress in the laboratory for geochronology of rocks using LA-MMS that is based on K-Ar radiogenic dating technique.

Sinha, Mahadeva P.↗
NASA NTRS2008

[Stardust Amines]

We investigated the abundances of amino acids and amines, as well as their enantiomeric composition in water extracts of comet Wild 2 exposed aerogel and aluminum foils returned by Stardust using liquid chromatography with UV fluorescence detection and time of flight-mass spectrometry (LC-FD/ToF-MS). A suite of amino acids and amines including glycine, L-alanine, methylamine (MA), and ethylamine (EA) were identified in the Stardust bulk aerogel. With the exception of MA and EA, all other primary amines detected in comet-exposed aerogels were also present in the aerogel witness tile that was not exposed to Wild 2, suggesting that most amines are terrestrial in origin. The enhanced abundances of MA, EA, and possibly glycine in comet-exposed aerogel compared to controls, coupled with MA to EA ratios (approx.1 to 2) that are distinct from preflight aerogels (approx.7 to lo), suggest that these amines were captured from Wild 2. The presence of cometary amines in Stardust material supports the hypothesis that comets were an important source of prebiotic organics on the early Earth. To better understand their origin, a systematic study of all these species with C, N, and H compound specific isotopic analysis (CSIA) via gas chromatography quadrupole mass spectrometry in with parallel with combustion isotope ratio mass spectrometry (GC-QMS/IRMS) is being conducted. We will discuss our latest C-CSIA measurements and what they indicate about the origin of the amino acids extracted from Stardust samples.

Dworkin, Jason P.↗
DOE OSTI2025

Cu-, Co-, and Zn-Based Metal–Organic Framework-Derived Nanoporous Ion Emitters for Picogram Level Analysis of Actinides

Thermal ionization mass spectrometry (TIMS) is often regarded as the preferred technique for trace-level isotopic analysis of actinides owing to its high sensitivity and absence of carry-over effects. However, actinide sample utilization efficiency (SUE) is typically low (<0.05%) without the use of activators or specialized loading approaches which can yield SUEs of >5%. To this effect, we investigate a series of metal–organic framework (MOF)-based nanoporous ion emitters (nano-PIEs) that show enhanced ionization of actinides when used in TIMS loading. We study the impact of physical and chemical properties of MOFs on TIMS SUEs using two families of MOFs that can be synthesized under similar reaction conditions. The structural and chemical properties of these MOFs can be systematically modified one at a time while keeping other features the same. This allows us to strategically investigate their impact on SUEs. The first family of MOFs considered in this study is Zeolitic Imidazole Frameworks (ZIFs) which are made using 2 methyl-imidazole as an organic linker with zinc (ZIF-8) and cobalt (ZIF-67) as metal centers. Additionally, the effect of morphology was also studied using Zn-based ZIF-L with a 2-dimensional structure. The second family of MOFs was synthesized using benzene-1,3,5-tricarboxylate (BTC) with copper (Cu-BTC) and zinc (Zn-BTC) as the metal center. Among the MOFs tested, Cu-BTC showed the highest SUE with an average SUE of 0.27 ± 0.15%, followed closely by Zn-BTC (0.24 ± 0.10%), ZIF-8 (0.17 ± 0.10%), and trailed by the other MOFs. When the MOFs were pyrolyzed in N 2 before loading, an apparent increase in the SUE was observed with ZIF-8 and Cu-BTC showing average SUEs of 0.25 ± 0.08% and 0.34 ± 0.13%, respectively, with the highest measured SUE of 0.53% for pyrolyzed Cu-BTC. In conclusion, this observed increase in SUE by up to an order of magnitude compared to bare filaments demonstrates the efficacy and potential of MOF-derived nano-PIEs for TIMS application.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS2009

Detection of Cometary Amines in Samples Returned by the Stardust Spacecraft

The delivery of amino acids to the early Earth by comets and their fragments could have been a significant source of the early Earth's prebiotic organic inventory that led to the emergence of life (Chyba and Sagan, 1992). Over 20 organic molecules including methane, ethane, ammonia, cyanic acid, formaldehyde, formamide, acetaldehyde, acetonitrile, and methanol have been identified by radio spectroscopic observations of the comae of comets Hale-Bopp and Hyakutake (Crovisier et al. 2004). These simple molecules could have provided the organic reservoir to allow the formation of more complex prebiotic organic compounds such as amino acids. After a 7-year mission, the Stardust spacecraft returned to Earth samples from comet Wild 2 on January 15, 2006 providing the opportunity to analyze the organic composition and isotopic distribution of cometary material with state-of-the-art laboratory instrumentation. The Preliminary Examination Team analyses of organics in samples returned by Stardust were largely focused on particles that impacted the collector aerogel and aluminum foil (Sandford et al. 2006). However, it is also possible that Stardust returned a "diffuse" sample of gas-phase organic molecules that struck the aerogel directly or diffused away from the grains after impact. To test this possibility, samples of Stardust flight aerogel and foil were carried through a hot water extraction and acid hydrolysis procedure to see if primary amine compounds were present in excess of those seen in controls. Here we report highly sensitive liquid chromatography time-of-flight mass spectrometry measurements of amino acids and amines in samples returned from a comet (Glavin et al. 2008). A suite of amino acids and amines including glycine, L-alanine, methylamine (MA), and ethylamine (EA) were identified in the Stardust bulk aerogel. With the exception of MA and EA, all other primary amines detected in comet-exposed aerogels were also present in the aerogel witness tile that was not exposed to Wild 2, suggesting that most amines are terrestrial in origin. However, the enhanced abundances of MA, EA, and possibly glycine in comet-exposed aerogel compared to controls, coupled with MA to EA ratios (1 to 2) that are distinct from preflight aerogels (7 to 10), suggest that these amines were captured from Wild 2. It is possible that MA and EA were formed on energetically processed icy grains containing methane, ethane, and ammonia. The presence of cometary amines in Stardust material supports the hypothesis that comets were an important source of prebiotic organics on the early Earth. To better understand their origin, a systematic compound specific carbon isotopic analysis (C-CSIA) via gas chromatography quadrupole mass spectrometry in with parallel with combustion isotope ratio mass spectrometry (GCQMS/ IRMS) is being conducted. We will discuss our latest C-CSIA measurements and what they indicate about the origin of amino acids extracted from Stardust samples.

Glavin, Daniel P.↗
NASA NTRS2010

Detection of Cometary Amines in Samples Returned by the Stardust Spacecraft

The delivery of amino acids to the early Earth by comets and their fragments could have been a significant source of the early Earth's prebiotic organic inventory that led to the emergence of life (Chyba and Sagan, 1992). Over 20 organic molecules including methane, ethane, ammonia, cyanic acid, formaldehyde, formamide, acetaldehyde, acetonitrile, and methanol have been identified by radio spectroscopic observations of the comae of comets Hale-Bopp and Hyakutake (Crovisier et al. 2004). These simple molecules could have provided the organic reservoir to allow the forn1ation of more complex prebiotic organic compounds such as amino acids. After a 7 -year mission, the Stardust spacecraft returned to Earth samples from comet Wild 2 on January 15, 2006 providing the opportunity to analyze the organic composition and isotopic distribution of cometary material with state-of-the-art laboratory instrun1entation. The Preliminary Examination Team analyses of organics in samples returned by Stardust were largely focused on particles that impacted the collector aerogel and aluminum foil (Sandford et al. 2006). However, it is also possible that Stardust returned a "diffuse" sample of gas-phase organic molecules that struck the aerogel directly or diffused away from the grains after impact. To test this possibility, samples of Stardust flight aerogel and foil were carried through a hot water extraction and acid hydrolysis procedure to see if primary amine compounds were present in excess of those seen in controls. Here we report highly sensitive liquid chromatography time-of-flight mass spectron1etry measurements of amino acids and amines in samples returned from a comet (Glavin et al. 2008). A suite of amino acids and amines including glycine, L-alanine, methylamine (MA), and ethylamine (EA) were identified in the Stardust bulk aerogel. With the exception of MA and EA, all other primary amines detected in comet-exposed aerogels were also present in the aerogel witness tile that was not exposed to Wild 2, suggesting that most amines are terrestrial in origin. However, the enhanced abundances of MA, EA, and possibly glycine in comet-exposed aerogel compared to controls, coupled with MA to EA ratios (1 to 2) that are distinct from preflight aerogels (7 to 10), suggest that these amines were captured from Wild 2. It is possible that MA and EA were formed on energetically processed icy grains containing methane, ethane, and ammonia. The presence of cometary amines in Stardust material supports the hypothesis that comets were an important source of pre biotic organics on the early Earth. To better understand their origin, a systematic compound specific carbon isotopic analysis (C-CSIA) via gas chromatography quadrupole mass spectrometry in with parallel with combustion isotope ratio mass spectrometry (GC-QMS/IRMS) is being conducted. We will discuss our latest C-CSIA measurements and what they indicate about the origin of amino acids extracted from Stardust samples.

Glavin, Daniel P.↗
DOE OSTI2025

Round Robin Analysis of Uranium Isotopics on Cotton Swipes Measured Using Microextraction-Based Sampling Versus Conventional Bulk Analysis

A comparison of microextraction sampling methods to directly analyze uranium isotopics on cotton swipes was performed concurrently with traditional bulk-processing methods. For the microextraction sampling approach, two different detection platforms were evaluated, a quadrupole-based inductively coupled plasma mass spectrometer (ICP-MS) and the liquid sampling-atmospheric pressure glow discharge (LS-APGD) coupled to an Orbitrap mass spectrometer. Results presented from this innovative sampling approach (i.e., microextraction) are compared with a more traditional approach employed for analysis of cotton-based environmental swipes, namely bulk ashing/digestion, separation, and subsequent analysis by high-precision multi-collector ICP-MS. Overall, the microextraction approach proved to be a reliable and accurate means to determine isotopic ratios of uranium collected on cotton swipes. The ICP-MS-based detection had relative standard deviations of <0.65% for the major isotopic determinations, whereas the LS-APGD-Orbitrap method had relative standard deviations of <3%. The percent relative difference for the 235 U/ 238 U ratios, in comparison to the expected values, was <1% for ICP-MS and <4% for the microplasma-Orbitrap method. Additionally, the microextraction ICP-MS accurately (<2%) and precisely (<5%) determined the minor isotopic compositions (i.e., 234 U/ 238 U and 236 U/ 238 U).

ICP-MS↗
NASA NTRS1992

Water in SNC meteorites - Evidence for a Martian hydrosphere

The Shergotty-Nakhla-Chassigny (SNC) meteorites, purportedly of Martian origin, contain 0.04 to 0.4 percent water by weight. Oxygen isotopic analysis can be used to determine whether this water is extraterrestrial or terrestrial. Such analysis reveals that a portion of the water is extraterrestrial and furthermore was not in oxygen isotopic equilibrium with the host rock. Lack of equilibrium between water and host rock implies that the lithosphere and hydrosphere of the SNC parent body formed two distinct oxygen isotopic reservoirs. If Mars was the parent body, the maintenance of two distinct reservoirs may result from the absence of plate tectonics on the planet.

Karlsson, Haraldur R.↗
NASA NTRS2012

Calibration and Sequence Development Status for the Sample Analysis at Mars Investigation on the Mars Science Laboratory

The measurement goals of the Sample Analysis at Mars (SAM) instrument suite on the "Curiosity" Rover of the Mars Science Laboratory (MSL) include chemical and isotopic analysis of organic and inorganic volatiles for both atmospheric and solid samples [1,2]. SAM directly supports the ambitious goals of the MSL mission to provide a quantitative assessment of habitability and preservation in Gale crater by means of a range of chemical and geological measurements [3]. The SAM FM combined calibration and environmental testing took place primarily in 2010 with a limited set of tests implemented after integration into the rover in January 2011. The scope of SAM FM testing was limited both to preserve SAM consumables such as life time of its electromechanical elements and to minimize the level of terrestrial contamination in the SAM instrument. A more comprehensive calibration of a SAM-like suite of instruments will be implemented in 2012 with calibration runs planned for the SAM testbed. The SAM Testbed is nearly identical to the SAM FM and operates in a ambient pressure chamber. The SAM Instrument Suite: SAM's instruments are a Quadrupole Mass Spectrometer (QMS), a 6-column Gas Chromatograph (GC), and a 2-channel Tunable Laser Spectrometer (TLS). Gas Chromatography Mass Spectrometry is designed for identification of even trace organic compounds. The TLS [5] secures the C, H, and O isotopic composition in carbon dioxide, water, and methane. Sieved materials are delivered from the MSL sample acquisition and processing system to one of68 cups of the Sample Manipulation System (SMS). 59 of these cups are fabricated from inert quartz. After sample delivery, a cup is inserted into one of 2 ovens for evolved gas analysis (EGA ambient to >9500C) by the QMS and TLS. A portion of the gas released can be trapped and subsequently analyzed by GCMS. Nine sealed cups contain liquid solvents and chemical derivatization or thermochemolysis agents to extract and transform polar molecules such as amino acids, nucleobases, and carboxylic acids into compounds that are sufficiently volatile to transmit through the GC columns. The remaining 6 cups contain calibrants. SAM FM Calibration Overview: The SAM FM calibration in the Mars chamber employed a variety of pure gases, gas mixtures, and solid materials. Isotope calibration runs for the TLS utilized 13C enriched C02 standards and 0 enriched CH4. A variety of fluorocarbon compounds that spanned the entire mass range of the QMS as well as C3-C6 hydrocarbons were utilized for calibration of the GCMS. Solid samples consisting of a mixture of calcite, melanterite, and inert silica glass either doped or not with fluorocarbons were introduced into the SAM FM cups through the SAM inlet funnel/tube system.

Mahaffy, Paul R.↗
NASA NTRS2019

Analyses of Aliphatic Aldehydes and Ketones in Carbonaceous Chondrites

Aliphatic aldehydes and ketones are essential building blocks for the synthesis of more complex organic compounds. Despite their potentially key role as precursors of astrobiologically important molecules, such as amino acids and carboxylic acids, this family of compounds has scarcely been evaluated in carbonaceous chondrites. The paucity of such analyses likely derives from the low concentration of aldehydes and ketones in the meteorites and from the currently used chromatographic methodologies that have not been optimized for meteorite analysis. In this work, we report the development of a novel analytical method to quantify the molecular distribution and compound-specific isotopic analysis of 29 aliphatic aldehydes and ketones. Using this method, we have investigated the molecular distribution and C-13-isotopic composition of aldehydes and ketones in 10 carbonaceous chondrites from the CI, CM, CR, and CV groups. The total concentration of carbonyl compounds ranged from 130 to 1000 nmol g(exp -1) of meteorite with formaldehyde, acetaldehyde, and acetone being the most abundant species in all investigated samples. The C-13-isotopic values ranged from -67 to +64‰ and we did not observe clear relationships between C-13-content and molecular weight. Accurately measuring the relative abundances, determining the molecular distribution and isotopic composition of chondritic organic compounds is central in assessing both their formation chemistry and synthetic relationships.

Organic carbon↗
NASA NTRS2011

Calibration of the Quadrupole Mass Spectrometer of the Sample Analysis at Mars Instrument Suite

The SAM suite of instruments on the "Curiosity" Rover of the Mars Science Laboratory (MSL) is designed to provide chemical and isotopic analysis of organic and inorganic volatiles for both atmospheric and solid samples. The mission of the MSL investigations is to advance beyond the successful search for aqueous transformation in surface environments at Mars toward a quantitative assessment of habitability and preservation through a series of chemical and geological measurements. The SAM suite was delivered in December 2010 (Figure 1) to the Jet Propulsion Laboratory for integration into the Curiosity Rover. We previously outlined the range of SAM solid and gas calibrations implemented or planned and here we discuss a specific set of calibration experiments to establish the response of the SAM Quadrupole Mass Spectrometer (QMS) to the four most abundant gases in the Martian atmosphere CO2, N2, Ar, and O2, A full SAM instrument description and calibration report is presently in preparation.

Mahaffy, P. R.↗
DOE OSTI2026

ORNL Report of Analysis for the Verification of NRMP CRM U030A

In support of the Certified Reference Material (CRM) program managed by the Nuclear Reference Material Program (NRMP), the Material Signatures and Isotopic Standards (MSIS) group of Oak Ridge National Laboratory (ORNL) was asked to prepare a set of CRM U030A units for use as standards for isotopic analysis using multicollector thermal ionization mass spectrometry (TIMS) and inductively coupled plasma mass spectrometry (ICP-MS) instruments. This report documents the results of the verification measurements performed on three randomly selected units by the MSIS group’s ISO/IEC 17025:2017 accredited operating procedure CSD-AM-CIMS-IN20, Determination of Uranium and Plutonium Isotopic Composition using Thermal Ionization Mass Spectrometry [1], and in accordance with the quality assurance plan as described in QAP-X-96-CSD/RML-001, Nuclear Analytical Chemistry Laboratory Section Quality Assurance Plan [2].

Mathew, Kattathu [Oak Ridge National Laboratory (O↗
NASA NTRS2008

Exploration of the Habitability of Mars with the SAM Suite Investigation on the 2009 Mars Science Laboratory

The 2009 Mars Science Laboratory (MSL) with a substantially larger payload capability that any other Mars rover, to date, is designed to quantitatively assess a local region on Mars as a potential habitat for present or past life. Its goals are (1) to assess past or present biological potential of a target environment, (2) to characterize geology and geochemistry at the MSL landing site, and (3) to investigate planetary processes that influence habitability. The Sample Analysis at Mars (SAM) Suite, in its final stages of integration and test, enables a sensitive search for organic molecules and chemical and isotopic analysis of martian volatiles. MSL contact and remote surface and subsurface survey Instruments establish context for these measurements and facilitate sample identification and selection. The SAM instruments are a gas chromatograph (GC), a mass spectrometer (MS), and a tunable laser spectrometer (TLS). These together with supporting sample manipulation and gas processing devices are designed to analyze either the atmospheric composition or gases extracted from solid phase samples such as rocks and fines. For example, one of the core SAM experiment sequences heats a small powdered sample of a Mars rock or soil from ambient to -1300 K in a controlled manner while continuously monitoring evolved gases. This is followed by GCMS analysis of released organics. The general chemical survey is complemented by a specific search for molecular classes that may be relevant to life including atmospheric methane and its carbon isotope with the TLS and biomarkers with the GCMS.

Mahaffy, P. R.↗
NASA NTRS1973

A component of primitive nuclear composition in carbonaceous meteorites

Oxygen isotope analysis of anhydrous high-temperature phases from carbonaceous meteorite chondrites indicates a high degree of O(17) and O(18) isotope depletion. The isotope decay is believed to be a result of nuclear rather than chemical processes caused by the admixture of a component consisting of almost pure O(16). It is theorized that this component may predate the solar system and may represent interstellar dust with a separate history of nucleosynthesis.

Clayton, R. N.↗
NASA NTRS1993

The EET87513 clast N: A CM2 fragment in an HED polymict breccia

Xenoliths of material resembling carbonaceous chondrites have been found in several HED polymict breccias. Most workers concluded that these clasts are related to CM2 meteorites on the basis of texture, bulk composition, and mineralogy. Data on clast N, a carbonaceous chondrite fragment from the howardite EET87513 large enough (approximately 4x5mm on the surface of the slab from which it was separated) to extract bulk samples for INAA and oxygen isotope analysis and to provide a thin section for electron microprobe, SEM, and TEM analysis is reported. Preliminary data for this clast were previously reported. INAA was performed at Oregon State University and bulk oxygen isotopic composition was determined at the University of Chicago. These data confirm that EET87513 clast N is a fragment of CM2 material.

Buchanan, P. C.↗
NASA NTRS1999

Anomalous Xenon in the Precambrian Nuclear Reactor in Okelobondo (Gabon): A Possible Connection to the Fission Component in the Terrestrial Atmosphere

Some CFF-Xe (Chemically Fractionated Fission Xenon), whose isotopic composition is established by simultaneous decay and migration of radioactive fission products, is probably present in the Earth's lithosphere, a conclusion based on available Xe data from various crustal and mantle rocks . Our recent isotopic analysis of Xe in alumophosphate from zone 13 of Okelobondo (southern extension of Oklo), along with the independent estimation of the isotopic composition of atmospheric fission Xe , supports the hypothesis that CFF-Xe was produced on a planetary scale. Additional information is contained in the original extended abstract.

Meshik, A. P.↗
DOE OSTI2024

FRAM In-Depth [Slides]

FRAM is an isotopic analysis code nominally designed for plutonium and uranium. It can also analyze other materials such as spent fuel (off all ages), medical isotopes.

07 ISOTOPE AND RADIATION SOURCES↗
NASA NTRS2012

Chromatographic, Spectroscopic and Mass Spectrometric Approaches for Exploring the Habitability of Mars in 2012 and Beyond with the Curiosity Rover

The Sample Analysis at Mars (SAM) suite of instruments on the Curiosity Rover of Mars Science Laboratory Mission is designed to provide chemical and isotopic analysis of organic and inorganic volatiles for both atmospheric and solid samples. The goals of the science investigation enabled by the gas chromatograph mass spectrometer and tunable laser spectrometer instruments of SAM are to work together with the other MSL investigations is to quantitatively assess habitability through a series of chemical and geological measurements. We describe the multi-column gas chromatograph system employed on SAM and the approach to extraction and analysis of organic compounds that might be preserved in ancient martian rocks.

Mahaffy, Paul↗