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NASA NTRS2001

AMINO ACID ANALYSES OF THE ANTARCTIC CM2 METEORITES ALH 83100 AND LEW 90500 USING LIQUID CHROMATOGRAPHY-TIME OF FLIGHT-MASS SPECTROMETRY

The investigation of organic compounds in primitive carbonaceous meteorites provides a record of the chemical processes that occurred in the early solar system. In particular, amino acids have been shown to be potential indicators in tracing the nature of carbonaceous chondrite parent bodies [ 13. The delivery of amino acids by carbonaceous chondrites to the early Earth could have been any important source of the Earth's prebiotic organic inventory [2]. Over 80 different amino acids have been detected in the Murchison CM2 meteorite, most of them completely non-existent in the terrestrial biosphere [3]. We have optimized a new liquid chromatography-time-of-flight-mass spectrometry (LC-ToF-MS) technique coupled with OPAMAC derivatization in order to detect amino acids in meteorite extracts by UV fluorescence and exact mass simultaneously. The detection limit of the LC-ToF-MS instrument for amino acids is at least 3 orders of magnitude lower than traditional GC-MS techniques. Here we report on the first analyses of amino acids and their enantiomeric abundances in the CM2 carbonaceous meteorites ALH 83100, LEW 90500, and Murchison using this new LC-ToF-MS instrument configuration. Amino acid analyses of any kind for the CM meteorite ALH 83100 have not previously been reported.

Glavin, D. P.↗

NASA NTRS2008

Simulation of a Miniature, Low-Power Time-of-Flight Mass Spectrometer for In Situ Analysis of Planetary Atmospheres

We are implementing nano- and micro-technologies to develop a miniaturized electron impact ionization mass spectrometer for planetary science. Microfabrication technology is used to fabricate the ion and electron optics, and a carbon nanotube (CNT) cathode is used to generate the ionizing electron beam. Future NASA planetary science missions demand miniaturized, low power mass spectrometers that exhibit high resolution and sensitivity to search for evidence of past and present habitability on the surface and in the atmosphere of priority targets such as Mars, Titan, Enceladus, Venus, Europa, and short-period comets. Toward this objective, we are developing a miniature, high resolution reflectron time-of-flight mass spectrometer (Mini TOF-MS) that features a low-power CNT field emission electron impact ionization source and microfabricated ion optics and reflectron mass analyzer in a parallel-plate geometry that is scalable. Charged particle electrodynamic modeling (SIMION 8.0.4) is employed to guide the iterative design of electron and ion optic components and to characterize the overall performance of the Mini TOF-MS device via simulation. Miniature (less than 1000 cubic centimeters) TOF-MS designs (ion source, mass analyzer, detector only) demonstrate simulated mass resolutions greater than 600 at sensitivity levels on the order of 10(exp -3) cps/molecule N2/cc while consuming 1.3 W of power and are comparable to current spaceflight mass spectrometers. Higher performance designs have also been simulated and indicate mass resolutions approximately 1000, though at the expense of sensitivity and instrument volume.

King, Todd T.↗

NASA NTRS2012

A Miniature Laser Desorption/Ionization Time-of-Flight Mass Spectrometer for in Situ Analysis of Mars Surface Composition and Identification of Hazard in Advance of Future Manned Exploration

Future landed missions to Mars will be guided by two strategic directions: (1) sample return to Earth, for comprehensive compositional analyses, as recommended by the 2011 NRC Planetary Decadal Survey; and (2) preparation for human exploration in the 2030s and beyond, as laid out by US space policy. The resultant mission architecture will likely require high-fidelity in situ chemical/organic sample analyses within an extremely constrained resource envelope. Both science goals (e.g., MEPAG Goal 1, return sample selection, etc.) as well as identification of any potential toxic and biological hazards to humans, must be addressed. Over the past several years of instrument development, we have found that the adaptable, compact, and highly capable technique of laser desorption/ionization time-of-flight mass spectrometry (LD-TOF-MS) has significant potential to contribute substantially to these dual objectives. This concept thus addresses Challenge Area 1: instrumentation and Investigation Approaches.

Getty, S. A.↗

NASA NTRS2012

Laser Time-of-Flight Mass Spectrometry for Future In Situ Planetary Missions

Laser desorption/ionization time-of-flight mass spectrometry (LD-TOF-MS) is a versatile, low-complexity instrument class that holds significant promise for future landed in situ planetary missions that emphasize compositional analysis of surface materials. Here we describe a 5kg-class instrument that is capable of detecting and analyzing a variety of analytes directly from rock or ice samples. Through laboratory studies of a suite of representative samples, we show that detection and analysis of key mineral composition, small organics, and particularly, higher molecular weight organics are well suited to this instrument design. A mass range exceeding 100,000 Da has recently been demonstrated. We describe recent efforts in instrument prototype development and future directions that will enhance our analytical capabilities targeting organic mixtures on primitive and icy bodies. We present results on a series of standards, simulated mixtures, and meteoritic samples.

Getty, S. A.↗

NASA NTRS2013

Two-step Laser Time-of-Flight Mass Spectrometry to Elucidate Organic Diversity in Planetary Surface Materials.

Laser desorption/ionization time-of-flight mass spectrometry (LD-TOF-MS) holds promise to be a low-mass, compact in situ analytical capability for future landed missions to planetary surfaces. The ability to analyze a solid sample for both mineralogical and preserved organic content with laser ionization could be compelling as part of a scientific mission pay-load that must be prepared for unanticipated discoveries. Targeted missions for this instrument capability include Mars, Europa, Enceladus, and small icy bodies, such as asteroids and comets.

Europa↗

NASA NTRS2016

A Fly-Through Mission Strategy Targeting Peptide as a Signature of Chemical Evolution and Possible Life in Enceladus Plumes

In situ detection of organic molecules in the extraterrestrial environment provides a key step towards better understanding the variety and the distribution of building blocks of life and it may ultimately lead to finding extraterrestrial life within the Solar System. Here we present combined results of two separate experiments that enable us to realize such in situ life signature detection from the deep habitats of the "Ocean World": a hydrothermal reactor experiment simulating complex organic synthesis and a simulated fly-through capture experiment of organic-bearing microparticles using silica aerogels, followed by subsequent analysis. Both experiments employ peptide as a plausible organics existing in Encleadus plume particles produced in its subsurface ocean. Recent laboratory hydrothermal experiments and a theoretical model on silica saturation indicated an on going hydrothermal reactions in subsurface Enceladus ocean. Given the porous chondritic origin of the core, it is likely that organic compounds originated by radiation chemistry such as amino acid precursors could have been provided, leached, and altered through widespread water-rock interactions. By using the same laboratory experimental setup from the latest water-rock interaction study, we performed amino acid polymerization experiments for 144 days and monitored the organic complexity changing over time. So far over 3,000 peaks up to the size of greater than 600 MW were observed through the analysis of capillary electrophoresis time-of-flight mass spectrometry (CE-TOF-MS) with an indication of amino acid derivatives and short peptides. Generally abiotic polymerization of enantiomeric amino acids results in forming stereoisomeric peptides with identical molecular weight and formula as opposed to homochiral biopolymers. Assuming Enceladus plume particles may contain a mixture of stereoisomeric peptides, we were able to distinguish 16 of the 17 stereoisomeric tripeptides as a test sample using capillary electrophoresis (CE) under optimized conditions. We further conducted Enceladus plume fly-through capture experiment by accelerating peptides soaked in rock particles up to a speed of 5.7 km/s and capturing with originally developed hydrophobic silica aerogels. Direct peptide extraction with acetonitrile-water followed by CE analysis led to detection of only but two stereoisomeric acidic peptide peaks, presenting the first run-through hypervelocuty impact sample analysis targeting peptides as key molecule to to understand the ongoing astrobiology on Enceladus.

organic molecules↗

NASA NTRS2016

Tandem Mass Spectrometry on a Miniaturized Laser Desorption Time-of-Flight Mass Spectrometer

Tandem mass spectrometry (MSMS) is a powerful and widely-used technique for identifying the molecular structure of organic constituents of a complex sample. Application of MSMS to the study of unknown planetary samples on a remote space mission would contribute to our understanding of the origin, evolution, and distribution of extraterrestrial organics in our solar system. Here we report on the realization of MSMS on a miniaturized laser desorption time-of-flight mass spectrometer (LD-TOF-MS), which is one of the most promising instrument types for future planetary missions. This achievement relies on two critical components: a curved-field reflectron and a pulsed-pin ion gate. These enable use of the complementary post-source decay (PSD) and laser-assisted collision induced dissociation (L-CID) MSMS methods on diverse measurement targets with only modest investment in instrument resources such as volume and weight. MSMS spectra of selected molecular targets in various organic standards exhibit excellent agreement when compared with results from a commercial, laboratory-scale TOF instrument, demonstrating the potential of this powerful technique in space and planetary environments.

Li, Xiang↗

NASA NTRS2016

Spaceborne Remote Sensing of Aerosol Type: Global Distribution, Model Evaluation and Translation into Chemical Speciation

It is essential to evaluate and refine aerosol classification methods applied to passive satellite remote sensing. We have developed an aerosol classification algorithm (called Specified Clustering and Mahalanobis Classification, SCMC) that assigns an aerosol type to multi-parameter retrievals by spaceborne, airborne or ground-based passive remote sensing instruments [1]. The aerosol types identified by our scheme are pure dust, polluted dust, urban-industrialdeveloped economy, urban-industrialdeveloping economy, dark biomass smoke, light biomass smoke and pure marine. We apply the SCMC method to inversions from the ground-based AErosol RObotic NETwork (AERONET [2]) and retrievals from the space-borne Polarization and Directionality of Earths Reflectances instrument (POLDER, [3]). The POLDER retrievals that we use differ from the standard POLDER retrievals [4] as they make full use of multi-angle, multispectral polarimetric data [5]. We analyze agreement in the aerosol types inferred from both AERONET and POLDER and evaluate GEOS-Chem [6] simulations over the globe. Finally, we use in-situ observations from the SEAC4RS airborne field experiment to bridge the gap between remote sensing-inferred qualitative SCMC aerosol types and their corresponding quantitative chemical speciation. We apply the SCMC method to airborne in-situ observations from the NASA Langley Aerosol Research Group Experiment (LARGE, [7]) and the Differential Aerosol Sizing and Hygroscopicity Spectrometer Probe (DASH-SP, [8]) instruments; we then relate each coarsely defined SCMC type to a sum of percentage of individual aerosol species, using in-situ observations from the Particle Analysis by Laser Mass Spectrometry (PALMS, [9]), the Soluble Acidic Gases and Aerosol (SAGA, [10]), and the High - Resolution Time - of - Flight Aerosol Mass Spectrometer (HR ToF AMS, [11]).

airborne↗

NASA NTRS2023

The Spatial Distribution of Soluble Organic Matter and Their Relationship to Minerals in the Asteroid (162173) Ryugu

We performed in-situ analysis on a ~1 mm-sized grain A0080 returned by the Hayabusa2 spacecraft from near-Earth asteroid (162173) Ryugu to investigate the relationship of soluble organic matter (SOM) to minerals. Desorption electrospray ionization-high resolution mass spectrometry (DESI-HRMS) imaging mapped more than 200 CHN, CHO, CHO–Na (sodium adducted), and CHNO soluble organic compounds. A heterogeneous spatial distribution was observed for different compound classes of SOM as well as among alkylated homologues on the sample surface. The A0080 sample showed mineralogy more like an Ivuna-type (CI) carbonaceous chondrite than other meteorites. It contained two different lithologies, which are either rich (lithology 1) or poor (lithology 2) in magnetite, pyrrhotite, and dolomite. CHN compounds were more concentrated in lithology 1 than in lithology 2; on the other hand, CHO, CHO–Na, and CHNO compounds were distributed in both lithologies. Such different spatial distribution of SOM is likely the result of interaction of the SOM with minerals, during precipitation of the SOM via fluid activity, or could be due to difference in transportation efficiencies of SOMs in aqueous fluid. Organic-related ions measured by time-of-flight secondary ion mass spectrometry (ToF–SIMS) did not coincide with the spatial distribution revealed by DESI-HRMS imaging. This result may be because the different ionization mechanism between DESI and SIMS, or indicate that the ToF–SIMS data would be mainly derived from methanol-insoluble organic matter in A0080. In the Orgueil meteorite, such relationship between altered minerals and SOM distributions was not observed by DESI-HRMS analysis and field-emission scanning electron microscopy, which would result from differences of SOM formation processes and sequent alteration process on the parent bodies or even on the Earth. Alkylated homologues of CHN compounds were identified in A0080 by DESI-HRMS imaging as observed in the Murchison meteorite, but not from the Orgueil meteorite. These compounds with a large C number were enriched in Murchison fragments with abundant carbonate grains. In contrast, such relationship was not observed in A0080, implying different formation or growth mechanisms for the alkylated CHN compounds by interaction with fluid and minerals on the Murchison parent body and asteroid Ryugu.

Ryugu↗

NASA NTRSDate not supplied

Quick and Correlative TOF-SIMS Analysis of Dispersoid Content in Powder Feedstock and Printed Oxide Dispersion Strengthened Alloys

Oxide dispersion strengthening (ODS) of metal alloys, when combined with additive manufacturing (AM), can be used to solve high-temperature material application problems. The performance of ODS materials is dependent on nano-scale oxide being distributed uniformly throughout the metal matrix; a homogenous distribution is critical to the creep and yield strength. Therefore, quantifying and analyzing these oxide nanoparticles is essential for ODS alloy development. Assessing the chemistry and morphology of dispersoids in a material can be conducted using a variety of X-ray and electron-based methods. Time of Flight Secondary Ion Mass Spectrometry (TOF-SIMS), which assesses chemical concentrations from ion masses, provides the necessary spatial resolution and avoids potential spectral overlap of all elements present. In this work, preparing ODS powder feedstock and Laser Powder Bed Fusion AM was conducted with a NiCoCr alloy and yttria dispersoid, mixed with a Resodyn resonance mixer and printed on an EOS M100 3D printer at NASA Glenn. TOF-SIMS was performed on a Physical Electronics NanoTOF TRIFT V TOF-SIMS at Case Western Reserve University. The TOF-SIMS results collected on the feedstock powder samples correspond to the qualitative interpretation of the homogeneity of the oxide coating on the metal powder from SEM images. This provides quantitative support to the qualitative microscopy images collected earlier in the process design phase. The variance in the yttrium distribution on the powder feedstock samples also correlated with the variance of the yttrium distribution detected in the printed samples. This correlation supported the hypothesis that an even coating of yttria on the metal powders contributes to an even distribution of yttria in the printed material.

Laura G. Wilson↗

NASA NTRS1991

Imaging analysis of LDEF craters

Two small craters in Al from the Long Duration Exposure Facility (LDEF) experiment tray A11E00F (no. 74, 119 micron diameter and no. 31, 158 micron diameter) were analyzed using Auger electron spectroscopy (AES), time-of-flight secondary ion mass spectroscopy (TOF-SIMS), low voltage scanning electron microscopy (LVSEM), and SEM energy dispersive spectroscopy (EDS). High resolution images and sensitive elemental and molecular analysis were obtained with this combined approach. The result of these analyses are presented.

Radicatidibrozolo, F.↗

NASA NTRS1995

Image and compositional characteristics of the LDEF Big Guy impact crater

A 5.2 mm crater in Al-metal represents the largest found on LDEF. We have examined this crater by field emission scanning electron microscopy (FESEM), energy dispersive spectroscopy (EDS) and time-of-flight/secondary ion mass spectroscopy (TOF-SIMS) in order to determine if there is any evidence of impactor residue. Droplet and dome-shaped columns, along with flow features, are evidence of melting. EDS from the crater cavity and rim show Mg, C, O and variable amounts of Si, in addition to Al. No evidence for a chondritic impactor was found, and it hypothesized that the crater may be the result of impact with space debris.

Bunch, T. E.↗

NASA NTRS1999

Teflon FEP Analyzed After Retrieval From the Hubble Space Telescope

During the Hubble Space Telescope (HST) Second Servicing Mission, 6.8 years after the telescope was deployed in low Earth orbit, degradation of unsupported Teflon FEP (DuPont; fluorinated ethylene propylene), used as the outer layer of the multilayer insulation (MLI) blankets, was evident as large cracks on the telescope light shield. A sample of the degraded outer layer (see the photograph) was retrieved during the second servicing mission and returned to Earth for ground testing and evaluation. Also retrieved was a Teflon FEP radiator surface from a cryogen vent cover that was exposed to the space environment on the aft bulkhead of the HST. NASA Goddard Space Flight Center directed the efforts of the Hubble Space Telescope MLI Failure Review Board, whose goals included determining the FEP degradation mechanisms. As part of the investigations into the degradation mechanisms, specimens retrieved from the first and second HST servicing missions, 3.6 and 6.8 years after launch, respectively, were characterized through exhaustive mechanical, optical, and chemical testing. Testing led by Goddard included scanning electron microscopy, optical microscopy, tensile testing, solar absorptance measurements, time-of-flight secondary ion mass spectroscopy (TOF-SIMS), Fourier transform infrared microscopy (m-FTIR), attenuated total reflectance infrared microscopy (ATR/FTIR), and x-ray diffraction (XRD). The NASA Lewis Research Center contributed significantly to the analysis of the retrieved HST materials by leading efforts and providing results of bend testing, surface microhardness measurements, x-ray photoelectron spectroscopy, solid-state nuclear magnetic resonance spectroscopy, and density measurements. Other testing was conducted by Nano Instruments, Inc., and the University of Akron.

Dever, Joyce A.↗

NASA NTRS2003

Investigation of isovaline enantiomeric excesses in CM meteorites using liquid chromatography time of flight mass spectrometry

The enantiomeric abundances of the alpha-dialkyl amino acid isovaline were measured in the CM2 meteorites Murchison and LEW 90500 using a new liquid chromatography-time of flight-mass spectrometry (LC-ToF-MS) technique coupled with OPA/NAC derivatization and UV fluorescence detection. Previous analyses of Murchison have shown that L-enantiomeric excesses of isovaline range from 0 to 15.2% with significant variation between meteorite fragments [1]. For this study, hot water extracts of interior fragments (> 2 cm from fusion crust) of the Murchison (USNM 6650.2, mass 6 g) and LEW 90500 (split 69, parent 1, mass 5 g) carbonaceous meteorites were analyzed. Enantiomeric excesses were measured using the single ion LC-ToF-MS trace for the OPA/NAC derivative of isovaline at d z 393.15 (Fig. 1). L-isovaline excesses in these meteorite samples ranged from 18.9 to 20.5% for Murchison and -0.5 to 3.0% for LEW 90500. The measured values for Murchison are the largest enantiomeric excesses for isovaline reported to date. The enantiomeric excesses of L-isovaline cannot be the result of interference from other C5 amino acid isomers present in the meteorites or terrestrial contamination from the landing site environments. The L-isovaline excesses in Murchison are inconsistent with the synthesis of all of the isovaline by the Strecker-cyanohydrin pathway on the CM meteorite parent body. The mechanism(s) for the formation of the enantiomeric asymmetry in isovaline in Murchison are currently unknown and it is not clear how the asymmetry of alpha-dialkyl amino acids could be transferred to the a-hydrogen protein amino acids common in all life on Earth today.

Glavin, Daniel P.↗

NASA NTRS2007

Fast Airborne Aerosol Size and Chemistry Measurements with the High Resolution Aerosol Mass Spectrometer during the MILAGRO Campaign

The concentration, size, and composition of non-refractory submicron aerosol (NR-PM(sub l)) was measured over Mexico City and central Mexico with a High-Resolution Time-of-Flight Aerosol Mass Spectrometer (HR-ToF-AMS) onboard the NSF/NCAR C-130 aircraft as part of the MILAGRO field campaign. This was the first aircraft deployment of the HR-ToF-AMS. During the campaign the instrument performed very well, and provided 12 s data. The aerosol mass from the AMS correlates strongly with other aerosol measurements on board the aircraft. Organic aerosol (OA) species dominate the NR-PM(sub l) mass. OA correlates strongly with CO and HCN indicating that pollution (mostly secondary OA, SOA) and biomass burning (BB) are the main OA sources. The OA to CO ratio indicates a typical value for aged air of around 80 microg/cubic m (STP) ppm(exp -1). This is within the range observed in outflow from the Northeastern US, which could be due to a compensating effect between higher BB but lower biogenic VOC emissions during this study. The O/C atomic ratio for OA is calculated from the HR mass spectra and shows a clear increase with photochemical age, as SOA forms rapidly and quickly overwhelms primary urban OA, consistent with Volkamer et al. (2006) and Kleinman et al. (2008). The stability of the OA/CO while O/C increases with photochemical age implies a net loss of carbon from the OA. BB OA is marked by signals at m/z 60 and 73, and also by a signal enhancement at large m/z indicative of larger molecules or more resistance to fragmentation. The main inorganic components show different spatial patterns and size distributions. Sulfate is regional in nature with clear volcanic and petrochemical/power plant sources, while the urban area is not a major regional source for this species. Nitrate is enhanced significantly in the urban area and immediate outflow, and is strongly correlated with CO indicating a strong urban source. The importance of nitrate decreases with distance from the city likely due to evaporation. BB does not appear to be a strong source of nitrate despite its high emissions of nitrogen oxides, presumably due to low ammonia emissions. NR-chloride often correlates with HCN indicating a fire source, although other sources likely contribute as well. This is the first aircraft study of the regional evolution of aerosol chemistry from a tropical megacity.

DeCarlo, P. F.↗

NASA NTRS2012

Nitrogen Incorporation in CH4-N2 Photochemical Aerosol Produced by Far UV Irradiation

Nitrile incorporation into Titan aerosol accompanying hydrocarbon chemistry is thought to be driven by extreme UV wavelengths (lambda < 120 nm) or magnetospheric electrons in the outer reaches of the atmosphere. Far UV radiation (120 - 200 nm), which is transmitted down to the stratosphere of Titan, is expected to affect hydrocarbon chemistry only and not initiate the formation of nitrogenated species. We have examined the chemical properties of photochemical aerosol produced at far UV wavelengths using a High-Resolution Time-of-Flight Aerosol Mass Spectrometer (HR-ToF-AMS), which allows for elemental analysis of particle-phase products. Our results show that aerosol formed from CH4/N2 photochemistry contains a surprising amount of nitrogen, up to 16% by mass, a result of photolysis in the far UV. The proportion of nitrogenated organics to hydrocarbon species is shown to be correlated with that of N2 in the irradiated gas. The aerosol mass greatly decreases when N2 is removed, indicating that N2 plays a major role in aerosol production. Because direct dissociation of N2 is highly improbable given the immeasurably low cross-section at the wavelengths studied, the chemical activation of N2 must occur via another pathway. Any chemical activation of N2 at wavelengths > 120 nm is presently unaccounted for in atmospheric photochemical models. We suggest that reaction with CH radicals produced from CH4 photolysis may provide a mechanism for incorporating N into the molecular structure of the aerosol. Further work is needed to understand the chemistry involved, as these processes may have significant implications for prebiotic chemistry on the early Earth and similar planets.

Trainer, Melissa G.↗

NASA NTRS2012

Comparison of Nitrogen Incorporation in Tholins Produced by FUV Irradiation and Spark Discharge

The discovery of very heavy ions (Coates et al., 2007) in Titan's thermosphere has dramatically altered our understanding of the processes involved in the formation of the complex organic aerosols that comprise Titan's characteristic haze. Before Cassini's arrival, it was believed that aerosol production began in the stratosphere where the chemical processes were predominantly initiated by FUV radiation. This understanding guided the design of Titan atmosphere simulation experiments. However, the energy environment of the thermosphere is significantly different than the stratosphere; in particular there is a greater flux of EUV photons and energetic particles available to initiate chemical reactions, including the destruction of N2. in the upper atmosphere. Using a High Resolution Time-of-Flight Aerosol Mass Spectrometer (HR-ToF-AMS), we have obtained in situ composition measurements of aerosol particles (so'called "tholins") produced in CH4/N2 gas mixtures subjected to either FUV radiation (deuterium lamp, 115-400 nm) (Trainer et al., 2012) or a spark discharge. A comparison of the composition of tholins produced using the two different energy sources will be presented, in particular with regard to the variation in nitrogen content of the two types of tholin. Titan's aerosols are known to contain significant amounts of nitrogen (Israel et al., 2005) and therefore understanding the role of nitrogen in the aerosol chemistry is important to further our knowledge of the formation and evolution of aerosols in Titan's atmosphere.

Horst, S. M.↗

NASA NTRSDate not supplied

Contamination, Transportation or Transmutation in LENR Material Analyses

LENR experiments using various loading and triggering mechanisms rely on a variety of elemental and isotopic assays to determine LENR effects. These assays include optical microscopy, Scanning Electron Microscopy with Energy Dispersive X-Ray Analysis (SEM/EDX), X-Ray Photoelectron Spectroscopy (XPS) and Transmission Electron Microscopy (TEM). All of these methods observe the surface of a material. By dissolving or vaporizing the sample, Inductively Coupled Plasma Optical Element Spectroscopy (ICP-OES) can determine elemental composition (ppb) or with mass spectroscopy, isotopes (ICP/MS). One can use a focused ion beam (FIB) to cut open a sample and observe the “cut” with either SEM/EDX, or Time-of-Flight Secondary Ion Mass Spectroscopy (TOF-SIMS). High Purity Gamma Ray Spectroscopy (HPGe) and alpha/ beta Liquid Scintillator spectroscopy can be used. We’ve employed these assay methods in our NASA GRC research under both the Advanced Energy Conversion and Lattice Confinement Fusion Projects. However, there are limitations associated with each of these methods ranging from handling contamination, instrumental limitations including sensitivity and field of view, and sample preparation.

Low Energy Nuclear Reactions↗