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Application of high resolution gas chromatography-mass spectrometry to the analysis of the pyrolysis products of isoprene.
High resolution gas chromatography combined with mass spectrometry applied to analysis of pyrolysis products of isoprene from 300 to 1000 degrees C
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.
Acquisition of a High-resolution Inductively Coupled Plasma Mass Spectrometer for Cosmochemical and Geochemical Research
The primary goal of our research in this program is to develop new techniques for the analysis of volatile trace elements in very small samples using inductively coupled plasma mass spectrometry (ICP-MS) in preparation for samples returned by the Stardust mission. The instrument that will serve as the basis of our experiments is the ELEMENT2 high-resolution ICP-MS. We have spent the past year designing the laboratory to house this instrument as well as space to store and prepare samples returned by the Stardust mission. Unfortunately, the location that we had initially selected for the instrument turned out to be insufficient for our needs. This was determined almost eight months into the first year of our funding cycle, after extensive work including the production of engineering drawings. However, during this time the Lunar and Planetary Laboratory was selected to lead Phoenix, the first Mars Scout mission. As a result of this award LPL purchased a new, 50,000 square foot building. We have acquired 1400 square feet of laboratory space in this new facility. Four-hundred square feet will be used for a class-100 clean room. This area is designated for storage and preparation of extraterrestrial materials. The additional 1000 square feet will house the ELEMENT2 ICP-MS and peripheral devices. This is an enormous amount of space for this instrument, but it provides plenty of room for expansion in the future. The ICP-MS and the clean room facilities have been purchased. The instrument has been delivered. The startup time for this instrument is relatively short and we expect to be collecting our first data by mid-summer.
Miniaturized Ion and Neutral Mass Spectrometer for CubeSat Atmospheric Measurements
To increase the number of single point in-situ measurements of thermosphere and exosphere ion and neutral composition and density, miniaturized instrumentation is in high demand to take advantage of the increasing platform opportunities available in the smallsat/cubesat industry. The INMS (Ion-Neutral Mass Spectrometer) addresses this need by providing simultaneous measurements of both the neutral and ion environment, essentially providing two instruments in one compact model. The 1.3U volume, 570 gram, 1.8W nominal power INMS instrument makes implementation into cubesat designs (3U and above) practical and feasible. With high dynamic range (0.1-500eV), mass dynamic range of 1-40amu, sharp time resolution (0.1s), and mass resolution of MdM16, the INMS instrument addresses the atmospheric science needs that otherwise would have required larger more expensive instrumentation. INMS-v1 (version 1) launched on Exocube (CalPoly 3U cubesat) in 2015 and INMS-v2 (version 2) is scheduled to launch on Dellingr (GSFC 6U cubesat) in 2017. New versions of INMS are currently being developed to increase and add measurement capabilities, while maintaining its smallsat/cubesat form.
Development of high resolution simulations of the atmospheric environment using the MASS model
Numerical simulations were performed with a very high resolution (7.25 km) version of the MASS model (Version 4.0) in an effort to diagnose the vertical wind shear and static stability structure during the Shuttle Challenger disaster which occurred on 28 January 1986. These meso-beta scale simulations reveal that the strongest vertical wind shears were concentrated in the 200 to 150 mb layer at 1630 GMT, i.e., at about the time of the disaster. These simulated vertical shears were the result of two primary dynamical processes. The juxtaposition of both of these processes produced a shallow (30 mb deep) region of strong vertical wind shear, and hence, low Richardson number values during the launch time period. Comparisons with the Cape Canaveral (XMR) rawinsonde indicates that the high resolution MASS 4.0 simulation more closely emulated nature than did previous simulations of the same event with the GMASS model.
Multi-Pass Quadrupole Mass Analyzer
Analysis of the composition of planetary atmospheres is one of the most important and fundamental measurements in planetary robotic exploration. Quadrupole mass analyzers (QMAs) are the primary tool used to execute these investigations, but reductions in size of these instruments has sacrificed mass resolving power so that the best present-day QMA devices are still large, expensive, and do not deliver performance of laboratory instruments. An ultra-high-resolution QMA was developed to resolve N2 +/CO+ by trapping ions in a linear trap quadrupole filter. Because N2 and CO are resolved, gas chromatography columns used to separate species before analysis are eliminated, greatly simplifying gas analysis instrumentation. For highest performance, the ion trap mode is used. High-resolution (or narrow-band) mass selection is carried out in the central region, but near the DC electrodes at each end, RF/DC field settings are adjusted to allow broadband ion passage. This is to prevent ion loss during ion reflection at each end. Ions are created inside the trap so that low-energy particles are selected by low-voltage settings on the end electrodes. This is beneficial to good mass resolution since low-energy particles traverse many cycles of the RF filtering fields. Through Monte Carlo simulations, it is shown that ions are reflected at each end many tens of times, each time being sent back through the central section of the quadrupole where ultrahigh mass filtering is carried out. An analyzer was produced with electrical length orders of magnitude longer than its physical length. Since the selector fields are sized as in conventional devices, the loss of sensitivity inherent in miniaturizing quadrupole instruments is avoided. The no-loss, multi-pass QMA architecture will improve mass resolution of planetary QMA instruments while reducing demands on the RF electronics for high-voltage/high-frequency production since ion transit time is no longer limited to a single pass. The QMA-based instrument will thus give way to substantial reductions of the mass of flight instruments.
Compositional Measurements of Saturn's Upper Atmosphere and Rings From Cassini INMS: An Extended Analysis of Measurements From Cassini's Grand Finale Orbits
The Cassini spacecraft's final orbits sampled Saturn's atmosphere and returned surprisingly complex mass spectra from the Ion and Neutral Mass Spectrometer (INMS). Signal returned from the instrument included native Saturn species, as expected, as well as a significant amount of signal attributed to vaporized ices and higher mass organics believed to be owing into Saturn's atmosphere from the rings. In this paper, we present an in-depth compositional analysis of the mass spectra returned from Cassini's last few orbits. We use a mass spectral deconvolution algorithm designed specifically to handle the complexities involved with unit resolution spaceflight mass spectrometry data to determine the relative abundance of species detected in the observations. We calculate the downward external flux and mass deposition rates of ring volatile species into Saturn's atmosphere and conclude that during these observations ring material was being deposited into Saturn's equatorial region at a rate on the order of 10(exp 4) kg/s.
Compositional Measurements of Saturn's Upper Atmosphere and Rings From Cassini INMS: An Extended Analysis of Measurements From Cassini's Grand Finale Orbits
The Cassini spacecraft's final orbits sampled Saturn's atmosphere and returned surprisingly complex mass spectra from the Ion and Neutral Mass Spectrometer (INMS). Signal returned from the instrument included native Saturn species, as expected, as well as a significant amount of signal attributed to vaporized ices and higher mass organics believed to be flowing into Saturn's atmosphere from the rings. In this paper, we present an in-depth compositional analysis of the mass spectra returned from Cassini's last few orbits. We use a mass spectral deconvolution algorithm designed specifically to handle the complexities involved with unit resolution spaceflight mass spectrometry data to determine the relative abundance of species detected in the observations. We calculate the downward external flux and mass deposition rates of ring volatile species into Saturn's atmosphere and conclude that during these observations ring material was being deposited into Saturn's equatorial region at a rate on the order of 10(exp 4) kg/s.
Optical resolution of D, L amino acids by gas chromatography and mass spectrometry.
Optical scanning and resolution of D, L amino acids by gas-liquid chromatography and mass spectrometry
Thermal detectors for high resolution spectroscopy
Cryogenic microcalorimeters can be made sensitive enough to measure the energy deposited by a single particle or X-ray photon with an accuracy of about one electron volt. It may also be possible to construct detectors of several-kilograms mass whose resolution is only a few times worse than this. Data from relatively crude test devices are in good agreement with thermal performance calculations, and a total system noise of 11 eV FWHM has been obtained for a silicon detector operating at 98 mK. Observations of 35 eV FWHM for 6-keV X-rays with a different device have been made.
High-resolution stellar vidicon spectrophotometry. I - Variable mass loss from Arcturus and the hypothesis of giant convective elements
High-resolution spectrophotometry of the variable Ca II K line in the K2 IIIp star Alpha Boo was performed with the McMath Solar Telescope at Kitt Peak National Observatory and an experimental SEC vidicon camera. The results are compared with Copernicus observations of the Mg II h and k lines and with earlier Ca II data. It is found that either of two states may typically occur in the Arcturus chromosphere. From comparison with the results of model calculations for expanding chromospheres, it is concluded that these correspond respectively to a 'normal' state in which the mass loss is less than one billionth of a solar mass per year and an 'abnormal' state in which the mass loss is about 8 billionths of a solar mass per year. In the latter case, the expansion velocity is around 13 km/s at optical depth unity in the K-line, which exceeds the local sound speed. It is suggested that the abnormal state represents the rise to the photosphere of a very large convective element, as hypothesized for red giants by Schwarzschild (1975).
NASA's Space Lidar Measurements of Earth and Planetary Surfaces
A lidar instrument on a spacecraft was first used to measure planetary surface height and topography on the Apollo 15 mission to the Moon in 1971, The lidar was based around a flashlamp-pumped ruby laser, and the Apollo 15-17 missions used them to make a few thousand measurements of lunar surface height from orbit. With the advent of diode pumped lasers in the late 1980s, the lifetime, efficiency, resolution and mass of lasers and space lidar all improved dramatically. These advances were utilized in NASA space missions to map the shape and surface topography of Mars with > 600 million measurements, demonstrate initial space measurements of the Earth's topography, and measured the detailed shape of asteroid. NASA's ICESat mission in Earth orbit just completed its polar ice measurement mission with almost 2 billion measurements of the Earth's surface and atmosphere, and demonstrated measurements to Antarctica and Greenland with a height resolution of a few em. Space missions presently in cruise phase and in operation include those to Mercury and a topographic mapping mission of the Moon. Orbital lidar also have been used in experiments to demonstrate laser ranging over planetary distances, including laser pulse transmission from Earth to Mars orbit. Based on the demonstrated value of the measurements, lidar is now the preferred measurement approach for many new scientific space missions. Some missions planned by NASA include a planetary mission to measure the shape and dynamics of Europa, and several Earth orbiting missions to continue monitoring ice sheet heights, measure vegetation heights, assess atmospheric CO2 concentrations, and to map the Earth surface topographic heights with 5 m spatial resolution. This presentation will give an overview of history, ongoing work, and plans for using space lidar for measurements of the surfaces of the Earth and planets.
Design and Demonstration of the Mars Organic Molecule Analyzer (MOMA) on the ExoMars 2018 Rover
The Mars Organic Molecule Analyzer (MOMA) investigation is a key astrobiology experiment scheduled to launch on the joint ESA-Roscosmos ExoMars 2018 rover mission. MOMA will examine the chemical composition of geological samples acquired from depths of up to two meters below the martian surface, where fragile organic molecules may be protected from destructive cosmic radiation and/or oxidative chemical reactions. The heart of the MOMA mass spectrometer subsystem (i.e., MOMA-MS) is a miniaturized linear ion trap (LIT) that supports two distinct modes of operation to detect: i) volatile and semi-volatile, low-to-moderate mass organics (less than or equal to 500 Da) via pyrolysis coupled with gas chromatography mass spectrometry (pyr/GCMS); and, ii) more refractory, moderate-to-high mass compounds (up to 1000 Da) via laser desorption (LDMS) at ambient Mars pressures. Additionally, the LIT mass analyzer enables selective ion trapping via multi-frequency waveform ion excitation (e.g., stored waveform inverse Fourier transform, or SWIFT), and structural characterization of complex molecules using tandem mass spectrometry (MSIMS). A high-fidelity Engineering Test Unit (ETU) of MOMAMS, including the LIT subassembly, dual-gun electron ionization source, micropirani pressure gauge, solenoid-driven aperture valve, redundant detection chains, and control electronics, has been built and tested at NASA GSFC under relevant operational conditions (pressure, temperature, etc.). Spaceflight qualifications of individual hardware components and integrated subassemblies have been validated through vibration, shock, thermal, lifetime, and performance evaluations. The ETU serves as a pathfinder for the flight model buildup, integration and test, as the ETU meets the form, fit and function of the flight unit that will be delivered to MPS in late 2015. To date, the ETU of MOMA-MS has been shown to meet or exceed all functional requirements, including mass range, resolution, accuracy, instrumental drift, and Iimit-of-detection specifications, thereby enabling the primary science objectives of the MOMA investigation and ExoMars 2018 mission.
Non-Targeted Direct Infusion Soluble Organic Analysis on a Tarda Meteorite Extract
The differences in chemistry, mineralogy, and structure of chondrites demonstrate thevariations in time/space of their forming regions in the solar nebula. In contrast, the variationof the organic reserves in the solar nebula is unclear. Furthermore, their subsequent evolutionof organic matter on the parent body is still under debate. In a previous study on Tagish Lake(C2 ungrouped) we showed that the primordial soluble organic matter (SOM) could bedistinguished from the parent body's secondary alteration threw mass distribution. This studywill show the Tarda meteorite SOM primordial distribution, using the model from ourprevious study. We discuss its organic reservoirs and secondary alteration effects. We alsocompare the character of the SOM with previously analysed Orgueil (CI). Sample and method: Tarda (fall, 2020) was classified as a C2 ungroup carbonaceouschondrite. Its bulk three oxygen isotope composition is distinct from other chondrite groupsbut similar to CI-chondrite-like and Yamato-type-like [1] values. We analysed themethanol/toluene extract using the high-resolution Orbitrap mass spectrometer at the Institutede Planétologie et d’Astrophysique Grenoble (IPAG) by directly injecting and ionizing theSOM and the solvent using the Heated Electrospray Ionization (HESI) source. After thespectra acquisition, the in-house developed post-processing data analysis tools, Attributor [2],was used. Preliminary Result: The SOM mass distribution of Tarda was well-fitted by the modelinterpreted as the primordial SOM distribution in Tagish lake. This common distributionpattern implies the presence of a common organic reservoir or SOM formation mechanism.Orgueil’s mass spectrum showed a more complex mass-distribution and seemed to be affectedby secondary processes. In contrast to the mass-distribution, SOM’s elemental abundance wasdistinct. The Tarda extract was enriched in S-bearing organic compounds which was incontrast to the Tagish Lake extract consisting of mostly CHNO elements. The presentationwill also discuss the application of our technique to Ryugu or Bennu samples. [1] Meteoriticalbulletin database [2] Orthous-Daunay, F. R. et al. (2019) Geochemical Journal, 53(1), 21-32
The Mean Seasonal Cycle in Relative Sea Level From Satellite Altimetry and Gravimetry
Satellite altimetry and gravimetry are used to determine the mean seasonal cycle in relative sea level, a quantity relevant to coastal flooding and related applications. The main harmonics (annual, semiannual, terannual) are estimated from 25 years of gridded altimetry, while several conventional altimeter “corrections” (gravitational tide, pole tide, and inverted barometer) are restored. To transform from absolute to relative sea levels, a model of vertical land motion is developed from a high-resolution seasonal mass inversion estimated from satellite gravimetry. An adjustment for annual geocenter motion accounts for use of a center-of-mass reference frame in satellite orbit determination. A set of 544 test tide gauges, from which seasonal harmonics have been estimated from hourly measurements, is used to assess how accurately each adjustment to the altimeter data helps converge the results to true relative sea levels. At these gauges, the median annual and semiannual amplitudes are 7.1 cm and 2.2 cm, respectively. The root-mean-square differences with altimetry are 3.24 and 1.17 cm, respectively, which are reduced to 1.93 and 0.86 cm after restoration of corrections and adjustment for land motion. Example outliers highlight some limitations of present-day coastal altimetry owing to inadequate spatial resolution: upwelling and currents off Oregon and wave setup at Minamitori Island.
Further analysis of the IRIS iron isotope experiment
The IRIS Fe isotope experiment was extended to atomic charges of Z = 19, with isotopic distributions for 500 events ranging from 18 to 28. Normalization of the detector response functions at Fe-56 produced a single well resolved peak at Sc-45, establishing the resolution and mass scale of the device over the entire charge region. The abundance distributions for the predominantly primary isotopes Ca-40, Fe-54, Fe-56, Ni-58, and Ni-60 do not indicate a large admixture of material with distinctly nonsolar abundances.