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NASA NTRS2016

Airborne In-Situ Measurements of Formaldehyde Over California: First Results from the Compact Formaldehyde Fluorescence Experiment (COFFEE) Instrument

Formaldehyde (HCHO) is one of the most abundant oxygenated volatile organic compounds (VOCs) in the atmosphere, playing a role multiple atmospheric processes. Measurements of HCHO can be used to help quantify convective transport, the abundance of VOCs, and ozone production in urban environments. The Compact Formaldehyde FluorescencE Experiment (COFFEE) instrument uses Non-Resonant Laser Induced Fluorescence (NR-LIF) to detect trace concentrations of HCHO as part of the Alpha Jet Atmospheric eXperiment (AJAX) payload. Developed at NASA GSFC, COFFEE is a small, low maintenance instrument with a sensitivity of 100 pptv and a quick response time (1 sec). The COFFEE instrument has been customized to fit in an external wing pod on the Alpha Jet aircraft based at NASA ARC. The instrument can operate over a broad range of altitudes, from boundary layer to lower stratosphere, making it well suited for the Alpha Jet, which can access altitudes from the surface up to 40,000 ft. Results of the first COFFEE science flights preformed over the California's Central Valley will be presented. Boundary layer measurements and vertical profiles in the tropospheric column will both be included. This region is of particular interest, due to its elevated levels of HCHO, revealed in satellite images, as well as its high ozone concentrations. In addition to HCHO, the AJAX payload includes measurements of atmospheric ozone, methane, and carbon dioxide. Formaldehyde is one of the few urban pollutants that can be measured from space. Plans to compare in-situ COFFEE data with satellite-based HCHO observations such as those from OMI (Aura) and OMPS (SuomiNPP) will also be presented.

ozone↗

NASA NTRS2016

Airborne In-Situ Measurements of Formaldehyde over California: First Results from the Compact Formaldehyde Fluorescence Experiment (COFFEE) Instrument

coffee↗

NASA NTRSDate not supplied

Strategies for Determining Safety of Fermented Foods Produced in Space

The BioNutrients experiments examine the feasibility of using microbially produced foods – yogurt, kefir, fermented food products– to supplement the current prepackaged food system to provide freshly synthesized nutrients and genetically engineered protein therapeutics to support crew health for sustainable and long duration crewed exploration. Safety of the products must be established as direct consumption of such products is a risk due to potential contamination with pathogenic organisms. Identifying pathogen contamination is particularly challenging as the fermenting cultures can mask the presence of contaminating organisms. Here we consider current methods of detecting coliforms, aerobic colonies, non-lactic acid bacteria, molds (yeasts), and specific pathogens including Staphylococcus aureus and salmonella. We also consider alternate and additional testing including sequencing and quantitative PCR. We investigate the use of the E-Nose developed by NASA Ames Research Center. This portable device senses volatile organic compounds in real time and can be trained to recognize “good” uncontaminated products from contaminated ones as a means of predicting food safety. Finally, we consider methods of in-flight pasteurization to increase safety and decrease overall microbial load of these products. This presentation will summarize testing status and outline the strategy that will be employed in the BioNutrients-3 ISS fermented foods experiment.

Natalie Ball↗

NASA NTRSDate not supplied

Strategies for Determining Safety of Fermented Foods Produced in Space

Food↗

NASA NTRS2008

Miniature Mass Spectrometers on Space and Planetary Missions

Space flight mass spectrometers contribute our understanding of the origin and evolution of our solar system and even of life itself. This fundamental role has motivated increasing interest in miniature mass spectrometry for planetary missions. Several remarkable new instruments are en route or under development to investigate the composition of planetary bodies such as Mars and comets. For instance, the Sample Analysis at Mars (SAM) suite on the 2009 Mars Science Laboratory (MSL) mission includes a quadrupole mass spectrometer with a sophisticated gas processing system as well as pyrolysis and chemical derivatization protocols for solid samples. Future missions will require even lighter, lower power, and yet more capable mass spectrometers, particularly to analyze samples in situ on planetary surfaces. We have been developing laser-based mass spectrometers for elemental and organic/molecular analysis of rock, ice, or fine particle samples. These typically use time-of-flight (TOF) mass analyzers, which are readily miniaturized and can detect both atomic species and complex organics that occur in a variety of planetary materials. For example, nonvolatile polycyclic aromatic hydrocarbons and kerogen-like macromolecular carbon are found in some carbonaceous meteorites, which derived from asteroid parent bodies. A single focused laser pulse is able to volatilize and ionize some of these compounds for direct TOF analysis. While this is possible without any sample preparation or contact, sensitivity and quantitative performance can improve significantly with some sample handling. As such we have also been examining robotic mechanisms and protocols to accompany space flight mass spectrometers. In addition, sensors in early development may significantly improve these capabilities, via use of techniques such as switchable polarity, ambient pressure, or resonant ionization; tandem mass spectrometry (TOF or ion trap); and chemical imaging.

Brinckerhoff, William↗

NASA NTRS2000

Multisorbent tubes for collecting volatile organic compounds in spacecraft air

The sampling capability of Tenax-TA tubes, used in the National Aeronautics and Space Administration's solid sorbent air sampler to trap and concentrate contaminants from air aboard spacecraft, was improved by incorporating two sorbents within the tubes. Existing tubes containing only Tenax-TA allowed highly volatile compounds to "break through" during collection of a 1.5 L air sample. First the carbon molecular sieve-type sorbents Carboxen 569 and Carbosieve S-III were tested for their ability to quantitatively trap the highly volatile compounds. Breakthrough volumes were determined with the direct method, whereby low ppm levels of methanol or Freon 12 in nitrogen were flowed through the sorbent tubes at 30 mL/min, and breakthrough was detected by gas chromatography. Breakthrough volumes for methanol were about 9 L/g on Carboxen 569 and 11 L/g on Carbosieve S-III; breakthrough volumes for Freon 12 were about 7 L/g on Carboxen 569 and > 26 L/g on Carbosieve S-III. Next, dual-bed tubes containing either Tenax-TA/Carbosieve S-III, Tenax-TA/Carboxen 569, or Carbotrap/Carboxen 569 to a 10-component gas mixture were exposed, in dry and in humidified air (50% relative humidity), and percentage recoveries of each compound were determined. The Tenax-TA/Carboxen 569 combination gave the best overall recoveries (75-114% for the 10 compounds). Acetaldehyde had the lowest recovery (75%) of the 10 compounds, but this value was still an improvement over either the other two sorbent combinations or the original single-sorbent tubes.

NASA Center JSC↗

NASA NTRSDate not supplied

A21I-1875: Leveraging TEMPO Formaldehyde Observations to Assess Surface Air Quality

Surface ozone (O3) pollution is detrimental to human health, crop yields, and ecosystem productivity. Ground-based ozone observations are sparse and surface ozone retrievals from space are challenging. The process of producing ozone from the oxidation of volatile organic compounds (VOCs) in the presence of nitrogen oxides (NOx) results in formaldehyde (HCHO), which can be observed from satellite and by surface-based remote sensing. From limited field campaign observations, column formaldehyde has been shown to exhibit a strong relationship with surface ozone and, therefore, could be an useful proxy for detecting unmonitored regions of elevated ozone pollution. The spatiotemporal characteristics of this relationship are explored using ground-based Pandora spectrometers and airborne remote sensing data with surface ozone monitors across the United States during recent field campaigns over major cities (TRACER-AQ and STAQS). We extend our analysis to take advantage of HCHO column observations from recently launched Tropospheric Emissions: Monitoring of Pollution (TEMPO), a geostationary satellite over North America. TEMPO observations show preliminary promise in mapping regions of elevated surface ozone from space using column HCHO. We demonstrate the use of column HCHO in assessing the strength of the surface monitoring network, and in detecting the extent of regional ozone exceedances.

Prajjwal Rawat↗

DOE OSTI2024

Tethered balloon system and High-Resolution Mass Spectrometry Reveal Increased Organonitrates Aloft Compared to the Ground Level

Atmospheric particles play critical roles in climate. However, significant knowledge gaps remain regarding the vertically resolved organic molecular-level composition of atmospheric particles due to aloft sampling challenges. To address this, we use a tethered balloon system at the Southern Great Plains Observatory and high-resolution mass spectrometry to, respectively, collect and characterize organic molecular formulas (MF) in the ground level and aloft (up to 750 m) samples. We show that organic MF uniquely detected aloft were dominated by organonitrates (139 MF; 54% of all uniquely detected aloft MF). Organonitrates that were uniquely detected aloft featured elevated O/C ratios (0.73 ± 0.23) compared to aloft organonitrates that were commonly observed at the ground level (0.63 ± 0.22). Unique aloft organic molecular composition was positively associated with increased cloud coverage, increased aloft relative humidity (~40% increase compared to ground level), and decreased vertical wind variance. Furthermore, 29% of extremely low volatility organic compounds in the aloft sample were truly unique to the aloft sample compared to the ground level, emphasizing potential oligomer formation at higher altitudes. Overall, this study highlights the importance of considering vertically resolved organic molecular composition (particularly for organonitrates) and hypothesizes that aqueous phase transformations and vertical wind variance may be key variables affecting the molecular composition of aloft organic aerosol.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2014

Searching for Reduced Carbon on the Surface of Mars: The SAM Combustion Experiment

The search for reduced carbon has been a major focus of past and present missions to Mars. Thermal evolved gas analysis was used by the Viking and Phoenix landers and is currently in use by the Sample Analysis at Mars (SAM) instrument suite on the Mars Science Laboratory (MSL) to characterize volatiles evolved from solid samples, including those associated with reduced organic species. SAM has the additional capability to perform a combustion experiment, in which a sample of Mars regolith is heated in the presence of oxygen and the composition of the evolved gases is measured using quadrupole mass spectrometry (QMS) and tunable laser spectrometry (TLS) [1]. Organics detection on the Martian surface has been complicated by oxidation and destruction during heating by soil oxidants [2], including oxychlorine compounds, and terrestrial organics in the SAM background contributed by one of the SAM wet chemistry reagents MTBSTFA (N-Methyl-N-tertbutyldimethylsilyl- trifluoroacetamide) [3,4]. Thermal Evolved Gas Analysis (TEGA) results from Phoenix show a mid temperature CO2 release between 400 C - 680 C speculated to be carbonate, CO2 adsorbed to grains, or combustion of organics by soil oxidants [5]. Low temperature CO2 evolutions (approx. 200 C - 400 C) were also present at all three sites in Gale Crater where SAM Evolved Gas Analysis (EGA) was performed, and potential sources include combustion of terrestrial organics from SAM, as well as combustion and/or decarboxylation either indigenous martian or exogenous organic carbon [4,6]. By performing an experiment to intentionally combust all reduced materials in the sample, we hope to compare the bulk abundance of CO2 and other oxidized species evolved by combustion to that evolved during an EGA experiment to estimate how much CO2 could be contributed by reduced carbon sources. In addition, C, O, and H isotopic compositions of CO2 and H2O measured by TLS can contribute information regarding the potential sources of these volatiles.

Stern, J. C.↗

DOE OSTI2024

Method Validation Summary for L16.2 AD-ISO-0015 for ISO-17025 / NFAC Applications

Methods for the analysis of semi-volatile organic compounds are employed at Savannah River National Laboratory (SRNL) for routine and non-routine samples from tank waste, process control, waste acceptance, and a wide array of other process and research samples. A method has been developed by SRNL, based on existing methods for semi-volatile analysis, for the analysis of nitroaromatic high explosives by gas chromatography / mass spectrometry in soils and sediments. Relative to past work performed at SRNL on nitroaromatic explosives, this developed, optimized, and validated method can achieve lower limits of detection and quantitation, greater precision, lower bias, higher linearity, and accuracy across a greater linear range.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

NASA NTRS1977

Analysis of volatile organic compounds

An apparatus and method are described for reproducibly analyzing trace amounts of a large number of organic volatiles existing in a gas sample. Direct injection of the trapped volatiles into a cryogenic percolum provides a sharply defined plug. Applications of the method include: (1) analyzing the headspace gas of body fluids and comparing a profile of the organic volatiles with standard profiles for the detection and monitoring of disease; (2) analyzing the headspace gas of foods and beverages and comparing the profile with standard profiles to monitor and control flavor and aroma; and (3) analyses for determining the organic pollutants in air or water samples.

Zlatkis, A.↗

DOE OSTI2019

Signaling from below: rodents select for deeper fruiting truffles with stronger volatile emissions

Many plant and fungal species use volatile organic compounds (VOCs) as chemical signals to convey information about the location or quality of their fruits or fruiting bodies to animal dispersers. Identifying the environmental factors and biotic interactions that shape fruit selection by animals is key to understanding the evolutionary processes that underpin chemical signaling. Using four Elaphomyces truffle species, we explored the role of fruiting depth, VOC emissions, and protein content in selection by five rodent species. We used stable isotope analysis of nitrogen (δ15N) in truffles to estimate fruiting depth, proton-transfer-reaction mass spectrometry to determine volatile emission composition, and nitrogen concentrations to calculate digestible protein of truffles. We coupled field surveys of truffle availability with truffle spore loads in rodent scat to determine selection by rodents. Despite presumably easier access to the shallow fruiting species, E. americanus (0.5-cm depth) and E. verruculosus (2.5-cm depth), most rodents selected for truffles fruiting deeper in the soil, E. macrosporus (4.1-cm depth) and E. bartlettii (5.0-cm depth). The deeper fruiting species had distinct VOC profiles and produced significantly higher quantities of odiferous compounds. Myodes gapperi (southern red-backed vole), a fungal specialist, also selected for truffles with high levels of digestible protein, E. verruculosus and E. macrosporus. Our results highlight the importance of chemical signals in truffle selection by rodents and suggest that VOCs are under strong selective pressures relative to protein rewards. Strong chemical signals likely allow detection of truffles deep within the soil and reduce foraging effort by rodents. Finally, for rodents that depend on fungi as a major food source, protein content may also be important in selecting truffles.

54 ENVIRONMENTAL SCIENCES↗

NASA NTRS2017

US Navy Submarine Sea Trial of the NASA Air Quality Monitor

For the past four years, the Air Quality Monitor (AQM) has been the operational instrument for measuring trace volatile organic compounds on the International Space Station (ISS). The key components of the AQM are the inlet preconcentrator, the gas chromatograph (GC), and the differential mobility spectrometer. Most importantly, the AQM operates at atmospheric pressure and uses air as the GC carrier gas, which translates into a small reliable instrument. Onboard ISS there are two AQMs, with different GC columns that detect and quantify 22 compounds. The AQM data contributes valuable information to the assessment of air quality aboard ISS for each crew increment. The U.S. Navy is looking to update its submarine air monitoring suite of instruments, and the success of the AQM on ISS has led to a jointly planned submarine sea trial of a NASA AQM. In addition to the AQM, the Navy is also interested in the Multi-Gas Monitor (MGM), which was successfully flown on ISS as a technology demonstration to measure major constituent gases (oxygen, carbon dioxide, water vapor, and ammonia). A separate paper will present the MGM sea trial results. A prototype AQM, which is virtually identical to the operational AQM, has been readied for the sea trial. Only one AQM will be deployed during the sea trial, but it is sufficient to detect the compounds of interest to the Navy for the purposes of this trial. A significant benefit of the AQM is that runs can be scripted for pre-determined intervals and no crew intervention is required. The data from the sea trial will be compared to archival samples collected prior to and during the trial period. This paper will give a brief overview of the AQM technology and protocols for the submarine trial. After a quick review of the AQM preparation, the main focus of the paper will be on the results of the submarine trial. Of particular interest will be the comparison of the contaminants found in the ISS and submarine atmospheres, as both represent closed environments. In U.K. submarine trials in the early 2000s, the submarine and ISS atmospheres were found to be remarkably similar.

Limero, Thomas↗

NASA NTRS1995

Monitoring Trace Contaminants in Air Via Ion Trap Mass Spectrometry

Recent passage of the Clean Air Act with its stricter regulation of toxic gas emissions, and the ever-growing number of applications which require faster turnaround times between sampling and analysis are two major factors which are helping to drive the development of new instrument technologies for in-situ, on-line, real-time monitoring. The ion trap, with its small size, excellent sensitivity, and tandem mass spectrometry capability is a rapidly evolving technology which is well-suited for these applications. In this paper, we describe the use of a commercial ion trap instrument for monitoring trace levels of chlorofluorocarbons (CFCs) and volatile organic compounds (VOCs) in air. A number of sample introduction devices including a direct transfer line interface, short column GC, and a cryotrapping interface are employed to achieve increasing levels of sensitivity. MS, MS/MS, and MS/MS/MS methods are compared to illustrate trade-offs between sensitivity and selectivity. Filtered Noise Field (FNF) technology is found to be an excellent means for achieving lower detection limits through selective storage of the ion(s) of interest during ionization. Figures of merit including typical sample sizes, detection limits, and response times are provided. The results indicate the potential of these techniques for atmospheric assessments, the High Speed Research Program, and advanced life support monitoring applications for NASA.

Palmer, Peter T.↗

NASA NTRS2018

Know Your Enemy - Implementation of Bioremediation within a Suspected DNAPL Source Zone Following High-Resolution Site Characterization at Contractors Road Heavy Equipment Area, Kennedy Space Center, Florida

The National Aeronautics and Space Administration (NASA), Kennedy Space Center (KSC), has adopted high-resolution site characterization (HRSC) sampling techniques during baseline sampling prior to implementation of remedies to confirm and refine the conceptual site model (CSM). HRSC sampling was performed at Contractors Road Heavy Equipment Area (CRHE) prior to bioremediation implementation to verify the extent of the trichloroethene (TCE) dense non-aqueous phase liquid (DNAPL) source area (defined as the area with TCE concentrations above 1% solubility) and its daughter product dissolved plume that had been identified during previous HRSC events. The results of HRSC pre-bioremediation implementation sampling suggested that the TCE source area was larger than originally identified during initial site characterization activities, leading to a design refinement to improve electron donor distribution and increase the likelihood of achieving remedial objectives. Approach/Activities: HRSC was conducted from 2009 through 2014 to delineate the vertical and horizontal extent of chlorinated volatile organic compounds (CVOCs) in the groundwater. Approximately 2,340 samples were collected from 363 locations using direct push technology (DPT) groundwater sampling techniques. Samples were collected from up to 14 depth intervals at each location using a 4-foot sampling screen. This HRSC approach identified a narrow (approx. 5 to 30 feet wide), approximately 3,000 square foot TCE DNAPL source area (maximum detected TCE concentration of 160,000 micrograms per liter [micro-g/L] at DPT sampling location DPT0225). Prior to implementation of a bioremediation interim measure, HRSC baseline sampling was conducted using DPT groundwater sampling techniques. Concentrations of TCE were an order of magnitude lower than previous reported (12,000 micro-g/L maximum at DPT sampling location DPT0225) at locations sampled adjacent to previous sampling locations. To further evaluate the variability in concentrations observed additional sampling was conducted in 2016. The results identified higher concentrations than originally detected within the previously defined source area and the presence of source zone concentrations upgradient of the previously defined source area (maximum concentration observed 570,000 micro-g/L). The HRSC baseline sampling data allowed for a revision of the bioremediation design prior to implementation. Bioremediation was implemented within the eastern portion of the source area in November and December 2016 and quarterly performance monitoring was completed in March and June 2017. Reductions in CVOC concentrations from baseline were observed at all performance monitoring wells in the treatment area, and by June 2017, an approximate 95% CVOC mass reduction was observed based on monitoring well sampling results. Results/Lessons Learned: The results of this project suggest that, due to the complexity of DNAPL source zones, HRSC during pre-implementation baseline sampling in the TCE source zone was an essential strategy for verifying the treatment area and depth prior to remedy implementation. If the upgradient source zone mass was not identified prior to bioremediation implementation, the mass would have served as a long-term source for the dissolved plume.

Chrest, Anne↗

DOE OSTI2026

Coupling of high-resolution mass spectrometer and photosynthesis system for comprehensive leaf volatile metabolite profiling

Background Leaf-level biogenic volatile organic compounds (BVOCs) emissions represent a major source of organic gases in the atmosphere, influencing both climate and air quality. These emissions are strongly driven by environmental perturbations, which affect individual plant- to ecosystem-level processes. Uncovering all the BVOCs and understanding how their emissions respond to altered environmental conditions provide critical insights into vegetation-driven changes in atmospheric chemistry. We developed a tandem instrumentation setup that integrates a proton transfer reaction time-of-flight mass spectrometer (PTR-ToF-MS) with parts-per-trillion detection limits and a photosynthetic infrared gas exchange system for the untargeted survey of all the BVOCs. This novel system enables simultaneous, real-time monitoring of BVOC emissions and photosynthetic parameters at the leaf level, offering new opportunities to disentangle the physiological and environmental drivers of VOC release. Furthermore, we established the VOC Analysis and Processing Optimization Resource (VAPOR), an open-access software tool designed for rapid data post-processing and the analysis of the variability of hundreds of BVOCs. We assessed the performance of the tandem system under varying background conditions, using standard gas mixtures and a range of environmental factors. Results Blank emissions were substantially lower for major BVOCs (e.g., isoprene) compared to those observed in plant emissions. Despite this, the observation of background-level VOCs highlights the importance of routinely acquiring and accounting for blank measurements in analyses using the coupled instrumentation. Introduction of known VOC concentrations to the system demonstrated a linear response across different compounds with varying molecular compositions, indicating minimal gas loss regardless of chemical moieties within the coupled instrumentation. We applied the optimized system to investigate the physiological mechanisms driving BVOC emissions across different genotypes of poplar and pennycress. The high mass resolution capabilities of the PTR-ToF-MS, coupled with comprehensive VAPOR-driven data analysis, enabled the identification of several important BVOCs, including methanol and methanethiol; these BVOCs displayed substantial variation across pennycress genotypes and showed concentrations ~ 100–350% higher than the blank. Moreover, isoprene emissions varied significantly among poplar genotypes grown in different potting media. Conclusions Tandem instrumentation offers a powerful tool for profiling volatile molecular markers and elucidating their genetic and environmental underpinnings. This approach enhances our ability to predict BVOC emissions in response to genotype by environmental interactions and contributes to a deeper understanding of vegetation responses to environmental changes.

Biogenic volatile organic compounds↗

NASA NTRS1992

A Volatile Organic Analyzer for Space Station - Description and evaluation of a gas chromatography/ion mobility spectrometer

An on-board Volatile Organic Analyzer (VOA), an essential component of the Environmental Health System (EHS) air-quality monitoring strategy, is described. The strategy is aimed at warning the crew and ground personnel if volatile compounds exceed safe exposure limits. The VOA uses a combination of gas chromatography (GC) and ion-mobility spectrometry (IMS) for environmental monitoring and analysis. It is concluded that the VOA dual-mode detection capability and the ion mobilities in the drift region are unique features that can assist in the resolution of coeluting GC peaks. The VOA is capable of accurately identifying and quantifying target compounds in a complex mixture.

Limero, Thomas↗

NASA NTRS2017

Monitoring of the Atmosphere on the International Space Station with the Air Quality Monitor

During the early years of human spaceflight, short duration missions allowed for monitoring of the spacecraft environment to be performed via archival sampling, in which samples were returned to Earth for analysis. With the construction of the International Space Station (ISS) and the accompanying extended mission durations, the need for enhanced, real-time monitors became apparent. The Volatile Organic Analyzer (VOA) operated on ISS for 7 years, where it assessed trace volatile organic compounds in the cabin air. The large and fixed-position VOA was eventually replaced with the smaller Air Quality Monitor (AQM). Since March 2013, the atmosphere of the U.S. Operating Segment (USOS) has been monitored in near real-time by a pair of AQMs. These devices consist of a gas chromatograph (GC) coupled with a differential mobility spectrometer (DMS) and currently target detection list of 22 compounds. These targets are of importance to both crew health and the Environmental Control and Life Support Systems (ECLSS) on ISS. Data is collected autonomously every 73 hours, though the units can be controlled remotely from mission control to collect data more frequently during contingency or troubleshooting operations. Due to a nominal three-year lifetime on-orbit, the initial units were replaced in February 2016. This paper will focus on the preparation and use of the AQMs over the past several years. A description of the technical aspects of the AQM will be followed by lessons learned from the deployment and operation of the first set of AQMs. These lessons were used to improve the already-excellent performance of the instruments prior to deployment of the replacement units. Data trending over the past several years of operation on ISS will also be discussed, including data obtained during a survey of the USOS modules. Finally, a description of AQM use for contingency and investigative studies will be presented.

Wallace William T.↗