Search NASA⌕ Search

SEARCH · Search NASA

Results for “mass spectrometry analysis”

Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 73 records · Page 4

Current Status of Martian Moons eXploration (MMX) Contamination Control and Curation Activity

Martian Moons eXploration (MMX) is a sample return mission from the Martian moon Phobos. The MMX spacecraft is scheduled to launch in 2026 and return to Earth in 2031. The main science goals of MMX are “to reveal the origin of the Martian moons and make progress in the understanding of planetary system formation and material transport in the solar system, and to observe processes that impact the circumplanetary and surface environments of Mars”. MMX has two sampling systems: coring (C)-sampler and pneumatic (P)-sampler and plans to bring back >10 g of Phobos sample. The retuned sample in the sample capsule will be transferred to the curation facility in ISAS/JAXA for sample curation and subsequent sample analysis. Contamination control of the sample return mission requires special care to prevent terrestrial contamination to the spacecraft, which would ruin the scientific value of the returned sample. Retaining the pristineness of the retuned sample is an important task of the MMX Curation and Sampler Science teams. The basis of the contamination control is (1) to minimize and understand the nature and amount of contaminants, (2) to perform contamination assessment and evaluate the effect of contaminants in the spacecraft on the retuned sample, (3) to employ a contamination knowledge (CK) material coupon in the spacecraft to identify the contaminants in the returned samples. In the MMX contamination control plan, the allowable contamination level for each contaminant is carefully defined. They are mostly set to be 1/1000 of the expected amount of each material in the returned sample and are divided into two main categories: organic and inorganic. The allowable atmospheric leakage rate to the sample container is also defined. The allowable contamination level of the organic materials is based on the composition of carbonaceous chondrites. The target contaminants are amino acids, aliphatic and aromatic hydrocarbons, carboxylic acids, etc. In case of the inorganic materials, the target contaminants are important elements to permit distinguishing the origin of the Martian moon by nucleosynthetic isotope anomalies (Cr, Ti, and Mo) and to reveal the evolution of the Martian moon by chronology (Hf, W, U, Pb, Rb, Sr, Sm, and Nd). The key instrument of contamination control in the sample return mission is the sampler system. The C-sampler has been developed by JAXA and the P-sampler was provided by Honeybee/NASA. In MMX, materials used in the two samplers (C- and P- sampler) were carefully selected to avoid potential contamination from the design stage of the system. The individual parts of the C-sampler FM (Flight Model) were thoroughly cleaned at the curation facility in ISAS/JAXA by the full-course cleaning procedure, which is an ultrasonic cleaning with organic solvents and ultrapure water in several steps. The equivalent level of cleaning was also carried out on the P-Samper FM as well by Honeybee Robotics in the USA. Now, MMX is in the critical phase for contamination control called ATLO: Assembly, Test, and Launch Operations. During the ATLO phase, sampler FM is constantly purged with nitrogen gas and maintained at positive pressure to prevent environmental contamination. The surrounding environments of the sampler FM are also simultaneously monitored using the CK Monitoring Coupon Set, which consists of several witness materials such as a glass petri dish, sapphire glass disk, and carbon adhesive tape (Figure 1). The detailed environmental assessment of each clean room used for the assembly and test of the sampler FM has also been conducted. This assessment includes microbial analysis, which was performed for OSIRIS-REx. Regarding the sample recovery and sample curation, we have started the designing of Sample Container Disassembling Instrument for the sample recovery from the sample container and the MMX curation chamber for sample curation. The curation protocol for the Phobos returned sample has also been discussed by the MMX Sample Analysis Working Team (SAWT). The MMX curation protocol consists of three phases: (1) quick analysis, (2) pre-basic characterization, and (3) basic characterization. (1) is extraction of the sample gas from the sample container and analysis by mass spectrometry, (2) is observation in bulk level, and (3) is observation in grain level and allocation of the sample aliquots. In parallel with the curation protocol, the returned sample undergoes preliminary examination for scientific investigations to achieve science goals. In addition, the CK witness plates made of sapphire glass are on board the sampler system. The CK witness plates will be recovered from the sampler system and analyzed by SAWT for the assessment of in-flight contamination.

Haruna Sugahara↗

An investigation of accelerating mode and decelerating mode constant-momentum mass spectrometry and their application to a residual gas analyzer

A theoretical analysis of constant momentum mass spectrometry was made. A maximum resolving power for the decelerating mode constant momentum mass spectrometer was shown theoretically to exist for a beam of ions of known energy. A vacuum system and an electron beam ionization source was constructed. Supporting electronics for a residual gas analyzer were built. Experimental investigations of various types of accelerating and decelerating impulsive modes of a constant momentum mass spectrometer as applied to a residual gas analyzer were made. The data indicate that the resolving power for the decelerating mode is comparable to that of the accelerating mode.

Ng, Y. S.↗

Developing Mass Spectrometry for Water Quantitation and Volatiles Analysis from In-Situ Regolith

With a revived focus to create a sustainable hu-man presence on the moon, and in preparation for future Mars exploration, it is imperative that all resources are utilized to their fullest potential [1]. In-Situ Resource Utilization (ISRU) will be critical for future mission success as it would enable in-dependent operation of missions while reducing the dependence on the complex supply chain created between the Earth, the moon and Mars. One of the most critical resources that has been identified for ISRU on the lunar surface is water [2]. Water is a versatile resource that can be used in various space operations, such as ra-diation shielding and conversion to oxygen (O2) for propellant [3,4]. One of the most water rich resources is thought to be within the regolith lo-cated in the permanently shadowed regions (PSR) of the Moon; several upcoming missions, such as PRIME-1 and VIPER, are already sched-uled to confirm this hypothesis [5,6]. However, there are currently no missions planned to quanti-fy the abudance of water at these regions. The quantity of water contained in the ice will inform and help the development of future ISRU plants and operation. Water and other volatile gases can be detect-ed upon controlled heating of icy lunar regolith for an accurate quantification of water. This method is similar to thermogravimetric analysis, which was used to analyze Apollo lunar regolith sam-ples. However, losses via sublimation/evaporation or contamination may have occurred with the samples due to the transit and exposure to the terrestrial environment. Furthermore, water would not be expected for these samples since they were not collected from a PSR. Thus, for more accurate results, icy lunar regolith should be ana-lyzed in situ to provide the most representative composition of both water and other volatile gas-es. The Light Water Analysis and Volatile Extract (LightWAVE) project aims to address this knowledge gap. A system has been developed to collect, heat and analyze evolved gases from lu-nar regolith on the lunar surface. The gases will be analyzed by a modified commercial off the shelf (COTS) residual gas analyzer (RGA) quad-rupole mass spectrometer. Evolved gases from heated regolith samples can be identified by the observed mass-to-charge (m/z) ratios, and the peak intensities correlate to the abundances of the observed gases for quantitation. Therefore, our group is developing a calibration methodology utilizing a COTS RGA to quantitate water from in-situ regolith samples on the lunar surface. The partial pressure of water and ideal gas law will be used to quantify the total water evolved from a regolith sample. Here we present our methodol-ogy for the design and calibration for water quan-titation using a COTS RGA.

Nilab Azim↗

Analysis of individual biological particles by mass spectrometry

A method is developed for the detection and identification of biological particles introduced in aerosol form into a quadrupole mass spectrometer. The bacterial aerosol is generated by nebulizing an ethanol suspension. The particles are introduced into the ion source of the mass spectrometer in the form of a beam, where they are individually volatilized on a V-type rhenium filament and ionized by electron impaction. It is shown that the average intensity of a mass peak is obtained from the pulse height distribution of about a thousand ion pulses from different particles. Pseudomonas putida, Bacillus subtilis, and Bacillus cereus are used in the studies. Differences between the relative intensities of mass peaks in the spectra from P. putida and B. subtilis are found and may provide a method for differentiation of microorganisms. The results for the two species agree reasonably well with those reported by Kistemaker et al. (1975) and Schulten et al. (1973). However, there exist some differences between the two spectra in the high mass range due to the difference in the pyrolysis conditions.

Sinha, M. P.↗

Low pressure gas flow analysis through an effusive inlet using mass spectrometry

A mass spectrometric method for analyzing flow past and through an effusive inlet designed for use on the tethered satellite and other entering vehicles is discussed. Source stream concentrations of species in a gaseous mixture are determined using a calibration of measured mass spectral intensities versus source stream pressure for standard gas mixtures and pure gases. Concentrations are shown to be accurate within experimental error. Theoretical explanations for observed mass discrimination effects as they relate to the various flow situations in the effusive inlet and the experimental apparatus are discussed.

Brown, David R.↗

High-Precision Measurement of Eu/Eu* in Geological Glasses via LA-ICP-MS Analysis

Elemental fractionation during laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) analysis has been historically documented between refractory and volatile elements. In this work, however, we observed fractionation between light rare earth elements (LREEs) and heavy rare earth elements (HREEs) when using ablation strategies involving large spot sizes (greater than 100 millimeters) and line scanning mode. In addition: (1) ion yields decrease when using spot sizes above 100 millimeters; (2) (Eu/Eu*)(sub raw) (i.e. Europium anomaly) positively correlates with carrier gas (He) flow rate, which provides control over the particle size distribution of the aerosol reaching the ICP; (3) (Eu/Eu*)(sub raw) shows a positive correlation with spot size, and (4) the changes in REE signal intensity, induced by the He flow rate change, roughly correlate with REE condensation temperatures. The REE fractionation is likely driven by the slight but significant difference in their condensation temperatures. Large particles may not be completely dissociated in the ICP and result in preferential evaporation of the less refractory LREEs and thus non-stoichiometric particle-ion conversion. This mechanism may also be responsible for Sm-Eu-Gd fractionation as Eu is less refractory than Sm and Gd. The extent of fractionation depends upon the particle size distribution of the aerosol, which in turn is influenced by the laser parameters and matrix. Ablation pits and lines defined by low aspect ratios produce a higher proportion of large particles than high aspect ratio ablation, as confirmed by measurements of particle size distribution in the laser induced aerosol. Therefore, low aspect ratio ablation introduces particles that cannot be decomposed and/or atomized by the ICP and thus results in exacerbated elemental fractionation. Accurate quantification of REE concentrations and Eu/Eu* requires reduction of large particle production during laser ablation. For the reference materials analyzed in this work, the 100 millimeters spot measurements of Eu/Eu* agreed with GeoRem preferred values within 3 percent. Our long-term analyses of Eu/Eu* in MPI-DING glass KL-2G and USGS glass BIR-1G were reproducible at 3 percent (2 RSD).

geological glasses↗

Mass spectrometry.

Review of the current state of mass spectrometry, indicating its unique importance for advanced scientific research. Mass spectrometry applications in computer techniques, gas chromatography, ion cyclotron resonance, molecular fragmentation and ionization, and isotope labeling are covered. Details are given on mass spectrometry applications in bio-organic chemistry and biomedical research. As the subjects of these applications are indicated alkaloids, carbohydrates, lipids, terpenes, quinones, nucleic acid components, peptides, antibiotics, and human and animal metabolisms. Particular attention is given to the mass spectra of organo-inorganic compounds, inorganic mass spectrometry, surface phenomena such as secondary ion and electron emission, and elemental and isotope analysis. Further topics include mass spectrometry in organic geochemistry, applications in geochronology and cosmochemistry, and organic mass spectrometry.

Burlingame, A. L.↗

Investigations of electret as a contamination control device

Thermoelectrets of polymers with stable surface charge on either side have been found to attract ions and charged particles to their surfaces. To assess their applicability to the control of atmospheric contamination, polytetraethylene (teflon) electrets are exposed to vapors coming from volatile mixtures over periods up to 90 min. Use is made of mass spectrometry for the analysis of teflon electret characteristics. It is found that even small quantities of the liquids in the mixture gives its characteristic mass spectra and that the peak height represents a measure for the quantity of the material collected over the electret surface, with the collected quantity being proportional to the duration of exposure.

Pillai, P. K. C.↗

Organic chemical analysis on a microscopic scale using two-step laser desorption/laser ionization mass spectrometry

The distribution of PAHs in the Allende meteorite has been measured using two-step laser desorption and laser multiphoton-ionization mass spectrometry. This method enables in situ analysis (with a spatial resolution of 1 mm or better) of selected organic molecules. Results show that PAH concentrations are locally high compared to the average concentration found by analysis of pulverized samples, and are found primarily in the fine-grained matrix; no PAHs were detected in the interiors of individual chondrules at the detection limit (about 0.05 ppm).

Kovalenko, L. J.↗

First Detection of Non-Chlorinated Organic Molecules Indigenous to a Martian Sample

The Sample Analysis at Mars (SAM) instrument onboard Curiosity can perform pyrolysis of martian solid samples, and analyze the volatiles by direct mass spectrometry in evolved gas analysis (EGA) mode, or separate the components in the GCMS mode (coupling the gas chromatograph and the mass spectrometer instruments). In addition, SAM has a wet chemistry laboratory designed for the extraction and identification of complex and refractory organic molecules in the solid samples. The chemical derivatization agent used, N-methyl-N-tert-butyldimethylsilyl- trifluoroacetamide (MTBSTFA), was sealed inside seven Inconel metal cups present in SAM. Although none of these foil-capped derivatization cups have been punctured on Mars for a full wet chemistry experiment, an MTBSTFA leak was detected and the resultant MTBSTFA vapor inside the instrument has been used for a multi-sol MTBSTFA derivatization (MD) procedure instead of direct exposure to MTBSTFA liquid by dropping a solid sample directly into a punctured wet chemistry cup. Pyr-EGA, Pyr-GCMS and Der-GCMS experiments each led to the detection and identification of a variety of organic molecules in diverse formations of Gale Crater.

Freissinet, C.↗

Discovery and Identification of Dimethylsilanediol as a Contaminant in ISS Potable Water

In September 2010, analysis of ISS potable water samples was undertaken to determine the contaminant(s) responsible for a rise of total organic carbon (TOC) in the Water Processor Assembly (WPA) product water. As analysis of the routine target list of organic compounds did not reveal the contaminant, efforts to look for unknown compounds were initiated, resulting in discovery of an unknown peak in the gas chromatography/mass spectrometry (GC/MS) analysis for glycols. A mass spectrum of the contaminant was then generated by concentrating one of the samples and analyzing it by GC/MS in full-scan mode. Although a computer match of the compound identity could not be obtained with the instrument database, a search with a more up-to-date mass spectral library yielded a good match with dimethylsilanediol (DMSD). Inductively coupled plasma/mass spectrometry (ICP/MS) analyses showed abnormally high silicon levels in the samples, confirming that the unknown compound(s) contained silicon. DMSD was then synthesized to confirm the identification and provide a standard to develop a calibration curve. Further confirmation was provided by external direct analysis in real time time of flight (DART TOF) mass spectrometry. To routinely test for DMSD in the future, a quantitative method was needed. A preliminary GC/MS method was developed and archived samples from various locations on ISS were analyzed to determine the extent of the contamination and provide data for troubleshooting. This paper describes these events in more detail as well as problems encountered in routine GC/MS analyses and the subsequent development of high performance liquid chromatography and LC/MS/MS methods for measuring DMSD.

Rutz, Jeffrey A.↗

Real-Time Quantitative Analysis of H2, He, O2, and Ar by Quadrupole Ion Trap Mass Spectrometry

The use of a quadrupole ion trap mass spectrometer for quantitative analysis of hydrogen and helium as well as other permanent gases is demonstrated. The customized instrument utilizes the mass selective instability mode of mass analysis as with commercial instruments; however, this instrument operates at a greater RF trapping frequency and without a buffer gas. With these differences, a useable mass range from 2 to over 50 Da is achieved, as required by NASA for monitoring the Space Shuttle during a launch countdown. The performance of the ion trap is evaluated using part-per-million concentrations of hydrogen, helium, oxygen and argon mixed into a nitrogen gas stream. Relative accuracy and precision when quantitating the four analytes were better than the NASA-required minimum of 10% error and 5% deviation, respectively. Limits of detection were below the NASA requirement of 25-ppm hydrogen and 100-ppm helium; those for oxygen and argon were slightly higher than the requirement. The instrument provided adequate performance at fast data recording rates, demonstrating the utility of an ion trap mass spectrometer as a real-time quantitative monitoring device for permanent gas analysis.

Ottens, Andrew K.↗

Differential thermal analysis and gas release studies of Apollo 11 samples.

The liquidus-solidus behavior of Apollo 11 lunar fines and the evolution characteristics of CO, nitrogen, He, Ne, and Ar were investigated by use of the combined techniques of high-vacuum differential thermal analysis (DTA) and mass spectrometry between 100 and 1500 C. The DTA thermogram has shown that the lunar fines undergo partial melting over a broad range of temperature from about 915 to 1300 C, with a significant initial melting of glassy and crystalline components within the fines at about 1140 C. The lunar material becomes a homogeneous melt at about 1300 C.

Wachi, F. M.↗

Rate constant for the reaction between OH and CS2 at 298 and 520 K

In an attempt to resolve discrepancies between published values of the rate constant for the reaction between the hydroxyl radical and carbon disulfide, the reaction has been studied in a discharge flow system by using resonance fluorescence for kinetic measurements and mass spectrometry for product analysis. On the basis of the measured rate constant for disappearance of OH, and measurements of the amount of carbonyl sulfide formed, it was estimated that for the reaction HO + CS2 yields HS + OCS, rate constant values are not greater than 3 x 10 to the -15th/cu cm per sec at 520 K and not greater than 7 x 10 to the -15th/cu cm per sec at 298 K, upper limits are specified because of the inability to isolate exclusively this reaction channel, and because of possible involvement of wall reactions. These results confirm the low values found for this rate constant in two very recent studies.

Leu, M.-T.↗