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NASA NTRS1999

Miniature Time-of-Flight Mass Spectrometer

Major advances must occur to protect astronauts from prolonged periods in near-zero gravity and high radiation associated with extended space travel. The dangers of living in space must be thoroughly understood and methods developed to reverse those effects that cannot be avoided. Six of the seven research teams established by the National Space Biomedical Research Institute (NSBRI) are studying biomedical factors for prolonged space travel to deliver effective countermeasures. To develop effective countermeasures, each of these teams require identification of and quantitation of complex pharmacological, hormonal, and growth factor compounds (biomarkers) in humans and in experimental animals to develop an in-depth knowledge of the physiological changes associated with space travel. At present, identification of each biomarker requires a separate protocol. Many of these procedures are complicated and the identification of each biomarker requires a separate protocol and associated laboratory equipment. To carry all of this equipment and chemicals on a spacecraft would require a complex clinical laboratory; and it would occupy much of the astronauts time. What is needed is a small, efficient, broadband medical diagnostic instrument to rapidly identify important biomarkers for human space exploration. The Miniature Time-Of- Flight Mass Spectrometer Project in the Technology Development Team is developing a small, high resolution, time-of-flight mass spectrometer (TOFMS) to quantitatively measure biomarkers for human space exploration. Virtues of the JHU/APL TOFMS technologies reside in the promise for a small (less than one cubic ft), lightweight (less than 5 kg), low-power (less than 50 watts), rugged device that can be used continuously with advanced signal processing diagnostics. To date, the JHU/APL program has demonstrated mass capability from under 100 to beyond 10,000 atomic mass units (amu) in a very small, low power prototype for biological analysis. Further, the electronic nature of the TOFMS output makes it ideal for rapid telemetry to earth for in-depth analysis by ground support teams.

Potember, Richard S.↗
NASA NTRS2001

Toward a Micro Gas Chromatograph/Mass Spectrometer (GC/MS) System

Miniature mass filters (e.g., quadrupoles, ion traps) have been the subject of several miniaturization efforts. A project is currently in progress at JPL to develop a miniaturized Gas Chromatograph/Mass Spectrometer (GC/MS) system, incorporating and/or developing miniature system components including turbomolecular pumps, scroll type roughing pump, quadrupole mass filter, gas chromatograph, precision power supply and other electronic components. The preponderance of the system elements will be fabricated using microelectromechanical systems (MEMS) techniques. The quadrupole mass filter will be fabricated using an X-ray lithography technique producing high precision, 5x5 arrays of quadrupoles with pole lengths of about 3 mm and a total volume of 27 cubic mm. The miniature scroll pump will also be fabricated using X-ray lithography producing arrays of scroll stages about 3 mm in diameter. The target detection range for the mass spectrometer is 1 to 300 atomic mass units (AMU) with are solution of 0.5 AMU. This resolution will allow isotopic characterization for geochronology, atmospheric studies and other science efforts dependant on the understanding of isotope ratios of chemical species. This paper will discuss the design approach, the current state-of-the art regarding the system components and the progress toward development of key elements. The full system is anticipated to be small enough in mass, volume and power consumption to allow in situ chemical analysis on highly miniaturized science craft for geochronology, atmospheric characterization and detection of life experiments applicable to outer planet roadmap missions.

Wiberg, D. V.↗
NASA NTRS2005

Lunar and Planetary Science XXXVI, Part 6

Contents include the following: A Model for Multiple Populations of Presolar Diamonds. Characterization of Martian North Polar Geologic Units Using Mars Odyssey THEMIS Data. Effect of Flow on the Internal Structure of the Martian North Polar Layered Deposits. Elemental Abundance Distributions in Basalt Clays and Meteorites: Is It a Biosignature? Early Results on the Saturn System from the Composite Infrared Spectrometer. NanoSIMS D/H Imaging of Isotopically Primitive Interplanetary Dust Particles. Presolar (Circumstellar and Interstellar) Phases in Renazzo: The Effects of Parent Body Processing. Catastrophic Disruption of Hydrated Targets: Implications for the Hydrated Asteroids and for the Production of Interplanetary Dust Particles. Chemical and Mineralogical Analyses of Particles from the Stratospheric Collections Coinciding with the 2002 Leonid Storm and the 2003 Comet Grigg-Skjellerup Trail Passage. An Analysis of the Solvus in the CaS-MnS System. ESA s SMART-1 Mission at the Moon: First Results, Status and Next Steps. Europa Analog Ice-splitting Measurements and Experiments with Ice-Hunveyor on the Frozen Balaton-Lake, Hungary. Chromium on Eros: Further Evidence of Ordinary Chondrite Composition. Dust Devil Tracks on Mars: Observation and Analysis from Orbit and the Surface. Spatial Variation of Methane and Other Trace Gases Detected on Mars: Interpretation with a General Circulation Model. Mars Water Ice and Carbon Dioxide Seasonal Polar Caps: GCM Modeling and Comparison with Mars Express Omega Observations. Component Separation of OMEGA Spectra with ICA. Clathrate Formation in the Near-Surface Environment of Titan. Space Weathering: A Proposed Laboratory Approach to Explaining the Sulfur Depletion on Eros. Sample Collection from Small Airless Bodies: Examination of Temperature Constraints for the TGIP. Sample Collector for the Hera Near-Earth Asteroid Sample Return Mission. A Rugged Miniature Mass-Spectrometer for Measuring Aqueous Geochemistry on Mars. Martian and Lunar Pyroxene Microstructures Studied by Single-Crystal X-Ray Diffraction.

Source record↗
NASA NTRS2001

Mass spectrometry in the U.S. space program: past, present, and future

Recent years have witnessed significant progress on the miniaturization of mass spectrometers for a variety of field applications. This article describes the development and application of mass spectrometry (MS) instrumentation to support of goals of the U.S. space program. Its main focus is on the two most common space-related applications of MS: studying the composition of planetary atmospheres and monitoring air quality on manned space missions. Both sets of applications present special requirements in terms of analytical performance (sensitivity, selectivity, speed, etc.), logistical considerations (space, weight, and power requirements), and deployment in perhaps the harshest of all possible environments (space). The MS instruments deployed on the Pioneer Venus and Mars Viking Lander missions are reviewed for the purposes of illustrating the unique features of the sample introduction systems, mass analyzers, and vacuum systems, and for presenting their specifications which are impressive even by today's standards. The various approaches for monitoring volatile organic compounds (VOCs) in cabin atmospheres are also reviewed. In the past, ground-based GC/MS instruments have been used to identify and quantify VOCs in archival samples collected during the Mercury, Apollo, Skylab, Space Shuttle, and Mir missions. Some of the data from the more recent missions are provided to illustrate the composition data obtained and to underscore the need for instrumentation to perform such monitoring in situ. Lastly, the development of two emerging technologies, Direct Sampling Ion Trap Mass Spectrometry (DSITMS) and GC/Ion Mobility Spectrometry (GC/IMS), will be discussed to illustrate their potential utility for future missions. c 2001 American Society for Mass Spectrometry.

NASA Discipline Environmental Health↗
NASA NTRS1992

The plasma instrumentation for the Galileo Mission

The Galileo Mission's plasma instrumentation package encompasses a nested set of four spherical-plate electrostatic analyzers and three miniature magnetic mass spectrometers which identify the composition of the positive ion plasmas; the spectrometers' energy range is species-dependent. Two instrument microprocessors allow in-flight implementation of operational modes by ground command that are tailored for such specific regimes as the magnetosheath and the plasma sheet of the environs of Jupiter. Observational objectives include field-aligned currents, 3D ion bulk flows, Galilean satellite pickup ions, and the spatial distributions of plasmas.

Frank, L. A.↗
NASA NTRS1993

A Low-cost, Lightweight, and Miniaturized Time-of-flight Mass Spectrometer (TOFMS)

Time-of-flight mass spectrometers (TOFMS) are commonly used for mass analysis and for the measurement of energy distributions of charged particles. For achieving high mass and energy resolution these instruments generally comprise long flight tubes, often as long as a few meters. This necessitates high voltages and a very clean environment. These requirements make them bulky and heavy. We have developed an instrument and calibration techniques that are based on the design principles of TOFMS. However, instead of one long flight tube it consists of a series of cylindrical electrostatic lenses that confine ions under study along the axis of the flight tube.

Srivastava, S. K.↗
NASA NTRS2009

Characterization of a Carbon Nanotube Field Emission Electron Gun for the VAPoR Miniaturized Pyrolysis-Time-of-Flight Mass Spectrometer

We are developing the VAPoR (Volatile Analysis by Pyrolysis of Regolith) instrument towards studying soil composition, volatiles, and trapped noble gases in the polar regions of the Moon. VAPOR will ingest a soil sample and conduct analysis by pyrolysis and time-of-flight mass spectrometry (ToF-MS). Here, we describe miniaturization efforts within this development, including a carbon nanotube (CNT) field emission electron gun that is under consideration for use as the electron impact ionization source for the ToF-MS.

Getty, Stephanie↗
NASA NTRS2002

Dual Source Mass Spectrometer and Sample Handling System

We present details of a miniature integrated time-of-flight mass spectrometer and sample handling system under development to address some of the needs for in situ sample analysis on landed missions. Additional information is contained in the original extended abstract.

Brinckerhoff, W. B.↗
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 NTRS2012

Compact Two-step Laser Time-of-Flight Mass Spectrometer for in Situ Analyses of Aromatic Organics on Planetary Missions

RATIONALE A miniature time-of-flight mass spectrometer has been adapted to demonstrate two-step laser desorption-ionization (LOI) in a compact instrument package for enhanced organics detection. Two-step LDI decouples the desorption and ionization processes, relative to traditional laser ionization-desorption, in order to produce low-fragmentation conditions for complex organic analytes. Tuning UV ionization laser energy allowed control ofthe degree of fragmentation, which may enable better identification of constituent species. METHODS A reflectron time-of-flight mass spectrometer prototype measuring 20 cm in length was adapted to a two-laser configuration, with IR (1064 nm) desorption followed by UV (266 nm) postionization. A relatively low ion extraction voltage of 5 kV was applied at the sample inlet. Instrument capabilities and performance were demonstrated with analysis of a model polycyclic aromatic hydrocarbon, representing a class of compounds important to the fields of Earth and planetary science. RESULTS L2MS analysis of a model PAH standard, pyrene, has been demonstrated, including parent mass identification and the onset o(tunable fragmentation as a function of ionizing laser energy. Mass resolution m/llm = 380 at full width at half-maximum was achieved which is notable for gas-phase ionization of desorbed neutrals in a highly-compact mass analyzer. CONCLUSIONS Achieving two-step laser mass spectrometry (L2MS) in a highly-miniature instrument enables a powerful approach to the detection and characterization of aromatic organics in remote terrestrial and planetary applications. Tunable detection of parent and fragment ions with high mass resolution, diagnostic of molecular structure, is possible on such a compact L2MS instrument. Selectivity of L2MS against low-mass inorganic salt interferences is a key advantage when working with unprocessed, natural samples, and a mechanism for the observed selectivity is presented.

Getty, Stephanie↗
NASA NTRS1979

Study and evaluation of impulse mass spectrometers for ion analysis in the D and E regions of the ionosphere

Theoretical and numerical analyses were made of planar, cylindrical and spherical electrode time-of-flight mass spectrometers in order to optimize their operating conditions. A numerical analysis of potential barrier gating in time-of-flight spectrometers was also made. The results were used in the design of several small mass spectrometers. These were constructed and tested in a laboratory space simulator. Detailed experimental studies of a miniature cylindrical electrode time of flight mass spectrometer and of a miniature hemispherical electrode time of flight mass spectrometer were made. The extremely high sensitivity of these instruments and their ability to operate at D region pressures with an open source make them ideal instruments for D region ion composition measurements.

Kendall, B. R.↗
NASA NTRS2009

Low-Pressure, Field-Ionizing Mass Spectrometer

A small mass spectrometer utilizing a miniature field ionization source is now undergoing development. It is designed for use in a variety of applications in which there are requirements for a lightweight, low-power-consumption instrument that can analyze the masses of a wide variety of molecules and ions. The device can operate without need for a high-vacuum, carrier-gas feed radioactive ionizing source, or thermal ionizer. This mass spectrometer can operate either in the natural vacuum of outer space or on Earth at any ambient pressure below 50 torr (below about 6.7 kPa) - a partial vacuum that can easily be reached by use of a small sampling pump. This mass spectrometer also has a large dynamic range - from singly charged small gas ions to deoxyribonucleic acid (DNA) fragments larger than 104 atomic mass units - with sensitivity adequate for detecting some molecules and ions at relative abundances of less than one part per billion. This instrument (see figure) includes a field ionizer integrated with a rotating-field mass spectrometer (RFMS). The field ionizer effects ionization of a type characterized as "soft" in the art because it does not fragment molecules or initiate avalanche arcing. What makes the "soft" ionization mode possible is that the distance between the ionizing electrodes is less than mean free path for ions at the maximum anticipated operating pressure, so that the ionizer always operates on the non-breakdown side of the applicable Paschen curve (a standard plot of breakdown potential on the ordinate and pressure electrode separation on the abscissa). The field ionizer in this instrument is fabricated by micromachining a submicron-thick membrane out of an electrically nonconductive substrate, coating the membrane on both sides to form electrodes, then micromachining small holes through the electrodes and membrane. Because of the submicron electrode separation, even a potential of only 1 V applied between the electrodes gives rise to an electric field with a strength of in excess of a megavolt per meter strong enough to ionize any gas molecules passing through the holes. An accelerator grid and an electrostatic deflector focus the ions from the field ionizer into the rotating-field cell of the RFMS. The potentials applied to the electrodes of the cell to generate the rotating electric field typically range from 1 to 13 V. The ions travel in well-defined helices within this cell, after which they are collected in a Faraday cup. The mass of most of the molecules reaching the Faraday cup decreases with increasing frequency of rotation of the electric field in the cell. Therefore, the frequency of rotation of the electric field is made to vary in order to scan through a desired range of ion masses: For example, lightweight gas molecules are scanned at frequencies in the megahertz range, while DNA and other large organic molecules are scanned at kilohertz frequencies.

Hartley, Frank↗
NASA NTRS1983

Developing mass spectrometric techniques for boundary layer measurement in hypersonic high enthalpy test facilities

Thermodynamic flow properties of gases in the boundary layer or the flowfield have been mainly deduced from pressures and temperatures measured on a model. However, further progress with respect to an understanding of these properties requires a more complete characterization of the layer including determination of the gas composition and chemistry. Most attempts to measure boundary layer chemistry involve the employment of a mass spectrometer and an associated gas sampling system. The three major limiting factors which must be addressed for species measurement in aerothermodynamic investigations on models at reentry stream velocities, are gas sampling effects, instrument limitations, and problems with data acquisition. The present investigation is concerned with a concentrated effort to quantitatively identify and correct for instrument and sampling system effects, and to develop a miniaturized high performance mass spectrometer for on-model real-time analysis of the boundary layer and its associated atmosphere.

Wood, G. M., Jr.↗
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 NTRS2001

Evaluating Mass Analyzers as Candidates for Small, Portable, Rugged Single Point Mass Spectrometers for Analysis of Permanent Gases

For Space Shuttle launch safety, there is a need to monitor the concentration Of H2, He, O2, and Ar around the launch vehicle. Currently a large mass spectrometry system performs this task, using long transport lines to draw in samples. There is great interest in replacing this stationary system with several miniature, portable, rugged mass spectrometers which act as point sensors which can be placed at the sampling point. Five commercial and two non-commercial analyzers are evaluated. The five commercial systems include the Leybold Inficon XPR-2 linear quadrupole, the Stanford Research (SRS-100) linear quadrupole, the Ferran linear quadrupole array, the ThermoQuest Polaris-Q quadrupole ion trap, and the IonWerks Time-of-Flight (TOF). The non-commercial systems include a compact double focusing sector (CDFMS) developed at the University of Minnesota, and a quadrupole ion trap (UF-IT) developed at the University of Florida.

Arkin, C. Richard↗
NASA NTRS2001

Evaluating Mass Analyzers as Candidates for Small, Portable, Rugged Single Point Mass Spectrometers for Analysis of Permanent Gases

For Space Shuttle launch safety, there is a need to monitor the concentration of H2, He, O2 and Ar around the launch vehicle. Currently a large mass spectrometry system performs this task, using long transport lines to draw in samples. There is great interest in replacing this stationary system with several miniature, portable, rugged mass spectrometers which act as point sensors which can be placed at the sampling point. Five commercial and two non-commercial analyzers are evaluated. The five commercial systems include the Leybold Inficon XPR-2 linear quadrupole, the Stanford Research (SRS-100) linear quadrupole, the Ferran linear quadrupole array, the ThermoQuest Polaris-Q quadrupole ion trap, and the IonWerks Time-of-Flight (TOF). The non-commercial systems include a compact double focusing sector (CDFMS) developed at the University of Minnesota, and a quadrupole ion trap (UF-IT) developed at the University of Florida. The System Volume is determined by measuring the entire system volume including the mass analyzer, its associated electronics, the associated vacuum system, the high vacuum pump and rough pump. Also measured are any ion gauge controllers or other required equipment. Computers are not included. Scan Time is the time required for one scan to be acquired and the data to be transferred. It is determined by measuring the time required acquiring a known number of scans and dividing by said number of scans. Limit of Detection is determined first by performing a zero-span calibration (using a 10-point data set). Then the limit of detection (LOD) is defined as 3 times the standard deviation of the zero data set. (An LOD of 10 ppm or less is considered acceptable.)

Arkin, C. Richard↗