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All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Determination of impurities in cubic boron nitride (cBN) by inductively coupled plasma mass spectrometry (ICPMS)

The phase stability of cBN is critically dependent on the content and amount of impurities present. While studies have shown qualitatively that the addition of certain impurities can either increase or decrease the cBN-hBN phase transition temperature, studies have yet to show this effect quantitatively. This is because analytical methods to characterize minor and trace impurities in cBN are currently lacking. To this end, we present flux fusion methods capable of fully digesting cBN samples for ICPMS analyses. The materials used in this study are commercially available cBN powders in three different sizes. Two types of fluxes (LiOH and NaOH·H 2 O) are utilized so that both Li and Na impurities can be determined. To ensure the accuracy of Si measurements, a column chromatography method has been developed to purify Si from flux materials in order to increase the amount of dissolved sample sent to the ICP. Detection limits have been determined using procedural blanks and are found to be below 20 μg/g for all 58 elements analyzed except for Si, for which the detection limit is 312 μg/g. Nonetheless, all cBN powders studied are found to have high Si impurity levels that are above detection limit. This study provides a much-needed analytical protocol to enable comprehensive screening of impurities in cBN.

36 MATERIALS SCIENCE↗
DOE OSTI2025

Quantum-enhanced detection of viral cDNA via luminescence resonance energy transfer using upconversion and gold nanoparticles

Abstract The COVID-19 pandemic has profoundly impacted global economies and healthcare systems, revealing critical vulnerabilities in both. In response, our study introduces a sensitive and highly specific detection method for cDNA, leveraging Luminescence Resonance Energy Transfer (LRET) between upconversion nanoparticles (UCNPs) and gold nanoparticles (AuNPs), and achieves a detection limit of 242 fM for SARS-CoV-2 cDNA. This innovative sensing platform utilizes UCNPs conjugated with one primer and AuNPs with another, targeting the 5′ and 3′ ends of the SARS-CoV-2 cDNA, respectively, enabling precise differentiation of mismatched cDNA sequences and significantly improving detection specificity. Through rigorous experimental analysis, we established a quenching efficiency range from 10.4 % to 73.6 %, with an optimal midpoint of 42 %, thereby demonstrating the superior sensitivity of our method. Our work uses SARS-CoV-2 cDNA as a model system to demonstrate the potential of our LRET-based detection method. This proof-of-concept study highlights the adaptability of our platform for future diagnostic applications. Instrumental validation confirms the synthesis and formation of AuNPs, addressing the need for experimental verification of the preparation of nanomaterial. Our comparative analysis with existing SARS-CoV-2 detection methods revealed that our approach provides a low detection limit and high specificity for target cDNA sequences, underscoring its potential for targeted COVID-19 diagnostics. This study demonstrates the superior sensitivity and adaptability of using UCNPs and AuNPs for cDNA detection, offering significant advances in rapid, accessible diagnostic technologies. Our method, characterized by its low detection limit and high precision, represents a critical step forward in developing next-generation biosensors for managing current and future viral outbreaks. By adjusting primer sequences, this platform can be tailored to detect other pathogens, contributing to the enhancement of global healthcare responsiveness and infectious disease control.

Esmaeili, Shahriar [Institute for Quantum Science ↗
NASA NTRS1992

Limits on detectability of mass loss from cool dwarfs

Recent spectroscopic evidence supports the theoretical expectation that certain cool dwarfs may have stellar winds with M-dot values several orders of magnitude larger than the solar rate. For large enough values of M-dot, the emission from the wind is expected to have a spectrum which, at low enough frequencies, becomes a power law, S(v) about v exp alpha with alpha about 0.7. Data from IRAS and VLA suggest that such a spectrum may in fact occur in certain M dwarfs: a key test of the wind spectrum would be provided if the stars could be detected at lambda about 1 mm. We show that the M-dot required to ensure power-law emission is a few times 10 exp -10 solar mass/yr. With M-dot of this order, fluxes at lambda about 1 mm would be tens of mJy. Using the James Clerk Maxwell Telescope, we have tested this prediction on several stars: the data are suggestive but are near the limits of detection. Confirmation of our estimates will be important for evolution and for interstellar medium (ISM) physics: if even a few percent of all M dwarfs are losing mass at the above rates, the mass balance of the ISM will be dominated by M dwarfs.

Mullan, D. J.↗
NASA NTRS1999

Chemical Sensors Based on IR Spectroscopy and Surface-Modified Waveguides

Sol-gel processing techniques have been used to apply thin porous films to the surfaces of planar infrared (IR) waveguides to produce widely useful chemical sensors. The thin- film coating serves to diminish the concentration of water and increase the concentration of the analyte in the region probed by the evanescent IR wave. These porous films are composed of silica, and therefore, conventional silica surface modification techniques can be used to give the surface a specific functional character. The sol-gel film was surface-modified to make the film highly hydrophobic. These sensors were shown to be capable of detecting non-polar organic analytes, such as benzonitrile, in aqueous solution with detection limits in the ppb range. Further, these porous sol-gel structures allow the analytes to diffuse into and out of the films rapidly, thus reaching equilibrium in less than ten seconds. These sensors are unique because of the fact that their operation is based on the measurement of an IR absorption spectrum. Thus, these sensors are able to identify the analytes as well as measure concentration with high sensitivity. These developments have been documented in previous reports and publications. Recently, we have also targeted detection of the polar organic molecules acetone and isopropanol in aqueous solution. Polar organics are widely used in industrial and chemical processes, hence it is of interest to monitor their presence in effluents or decontamination process flows. Although large improvements in detection limits were expected with non-polar organic molecules in aqueous solutions using very hydrophobic porous sol-gel films on silicon attenuated total reflectance (Si ATR) waveguides, it was not as clear what the detection enhancements might be for polar organic molecules. This report describes the use of modified sol-gel-coated Si ATR sensors for trace detection and quantitation of small polar organic molecules in aqueous solutions. The detection of both acetone and isopropanol molecules in aqueous solution has been previously reported for chalcogenide fiber optic sensors. The sol-gel film was produced using a mixture of ethyltriethoxysilane and tetraethoxysilane and the surface modification was carried out using trimethylchlorosilane. We have demonstrated that this film concentrates the target polar analytes from aqueous solution in the region probed by the evanescent wave to improve detection limits by as much as a factor of 450.

Lopez, Gabriel P.↗
NASA NTRS2017

The Role of Carbon in Core Formation Under Highly Reducing Conditions With Implications for the Planet Mercury

Results from the MErcury Surface, Space ENvironment, GEochemistry and Ranging (MESSENGER) spacecraft have shown elevated abundances of carbon on the surface of Mercury. Furthermore, the X-Ray Spectrometer on board MESSENGER measured elevated abundances of sulfur and low abundances of iron, suggesting the planet's oxygen fugacity (fO2) is several log10 units below the Iron-Wüstite (IW) buffer. Similar to the role of other volatiles (e.g. sulfur) on highly reducing planetary bodies, carbon is expected to behave differently than it would under higher fO2. As discussed by Nittler et al. and Hauck et al., under such highly reducing conditions, the majority of the iron partitions into the core. On Mercury, this resulted in a relatively large core and a thin mantle. Using a composition similar to the largest volcanic field on the planet (the northern volcanic plains), Vander Kaaden and McCubbin conducted sink-float experiments to determine the density of melts and minerals on Mercury. They showed that graphite would be the only buoyant mineral in a mercurian magma ocean. Therefore, Vander Kaaden and McCubbin proposed a possible primary flotation crust on the planet composed of graphite. Concurrently, Peplowski et al. used GRS data from MESSENGER to show an average northern hemisphere abundance of C on the planet of 1.4 +/- 0.9 wt%. However, as this result was only at the one-sigma detection limit, possible carbon abundances at the three-sigma detection limit for Mercury range from 0 to 4.1 wt% carbon. Additionally, Murchie et al. investigated the possible darkening agent on Mercury and concluded that coarse-grained graphite could darken high reflectance plains to the low reflectance material. To further test the possibility of elevated abundances of carbon in Mercury's crust, Peplowski et al. used the low-altitude MESSENGER data to show that carbon is the only material consistent with both the visible to near-infrared spectra and the neutron measurements of low reflectance material on Mercury, confirming that C is the primary darkening agent on Mercury. Confirmation of carbon on the planet prompts many questions regarding the role of carbon during the differentiation and evolution of Mercury. Given the elevated abundances of both S and C on Mercury's surface, it begs the question, what is the core composition of the planet? This study seeks to understand the impact of C as a light element on potential core compositions on Mercury.

Vander Kaaden, Kathleen E..↗
NASA NTRS2013

Direct Imaging Search for Extrasolar Planets in the Pleiades

We carried out an imaging survey for extrasolar planets around stars in the Pleiades (125 Myr, 135 pc) in the H and K(sub S) bands using HiCIAO combined with adaptive optics, AO188, on the Subaru telescope. We found 13 companion candidates fainter than 14.5 mag in the H band around 9 stars. Five of these 13 were confirmed to be background stars by measurement of their proper motion. One was not found in the second epoch observation, and thus was not a background or companion object. One had multi-epoch images, but the precision of its proper motion was not sufficient to conclude whether it was a background object. Four other candidates are waiting for second-epoch observations to determine their proper motion. Finally, the remaining two were confirmed to be 60 M(sub J) brown dwarf companions orbiting around HD 23514 (G0) and HII 1348 (K5), respectively, as had been reported in previous studies. In our observations, the average detection limit for a point source was 20.3 mag in the H band beyond 1.′′ 5 from the central star. On the basis of this detection limit, we calculated the detection efficiency to be 90% for a planet with 6 to 12 Jovian masses and a semi-major axis of 50–1000 AU. For this reason we extrapolated the distribution of the planet mass and the semi-major axis derived from radial velocity observations, and adopted the planet evolution model Baraffe et al. (2003, A&A, 402, 701). Since there was no detection of a planet, we estimated the frequency of such planets to be less than 17.9% (2 sigma) around one star of the Pleiades cluster.

extrasolar planets↗
NASA NTRS2004

A Search for Coronal Emission at the Bottom of the Main-Sequence: Stars and Brown Dwarf Candidates with Spectral Types Later than M7 and the Rotation-Activity Relation

This program intended to test whether the lowest mass stars at the bottom end of the main sequence and the lower mass brown dwarfs have coronae. If they have coronae, what are the coronal characteristics and what drives them? In the classical dynamo picture, the closed magnetic loop structure is generated near the boundary of the convective envelope and the radiative core. Stars with mass below 0.30 Msun however are fully convective, and the nature of the dynamo responsible for the generation of the coronae in this regime is poorly understood. Previous results from the ROSAT mission (e.g., Fleming et al. 1993, 1995; Schmitt et al. 1995) had confirmed three very important characteristics of M-star coronae: (1) a very high percentage of all M dwarfs have coronae (of order 85% in the local 7 pc sample), (2) those M dwarfs showing high chromospheric activity, such as having the Balmer series in emission or large/numerous optical flaring, indeed exhibit the highest coronal activity, and (3) that the maximum saturation boundary in X-ray luminosity, which amounts to 0.0001-0.001 for Lx/Lbol for the dMe stars, extends down to the current detection limit, through spectral types M7. It was likely that the incompleteness noted for result (1) above was simply a detection limit problem; for more distant sources, the X-ray fainter dM stars will drop below detection thresholds before the more X-ray luminous dMe stars. The latest stars for which direct detection of the corona had been successful were of spectral type dM7 (e.g., VB8, LHS 3003). This program proposed to obtain ROSAT HRI observations for a large number of the coolest known (at that time) stars at the bottom of the main-sequence, which had spectral types of M9 or later. Three stars were approved for observations with ROSAT-HRI totaling 180 ksec. The goal was to obtain X-ray detections or low upper limits for the three approved stars.

Stringfellow, Guy↗
DOE OSTI2025

Search for Postinflationary QCD Axions with a Quantum-Limited Tunable Microwave Receiver

A search for cosmological axions has been performed by scanning a frequency region of 38 MHz centered at about 10.2 GHz, corresponding to an axion mass 𝑚 𝑎 ≃ 42 μ ⁢eV. The QUAX experimental apparatus, a haloscope comprised of a 1-liter volume tunable cavity immersed in an 8 T magnetic field and a quantum-limited detection chain, set limits on the axion-photon coupling at the 10 −14 GeV −1 level. As no signal candidate has been observed, viable hadronic axion models are ruled out in a currently preferred postinflationary region 𝑚 𝑎 > 40 μ ⁢eV.

Sardo Infirri, Giosue [INFN, Sezione di Padova; Un↗
NASA NTRS1986

Elemental analysis of a comet nucleus by passive gamma ray spectrometry from a penetrator

The Comet Rendezvous Asteroid Flyby (CRAF) spacecraft, to be launched in 1991, was designed to study the physical and chemical properties of cometary and asteroid bodies. It is proposed that these properties can be determined by utilizing a penetrator experiment delivery system aboard the CRAF, which would deliver a passive gamma ray spectrometer to the comet and determine the composition of subsurface materials. Results of calculations for a model comet (50 percent CI carbonaceous chrondrite, 50 percent ices) provide data on the expected gamma ray fluxes, the minimum detectable limits, and the detection uncertainties for 35 isotopes. These results confirm that this technique can determine the composition of both the rocky and ice components, and the rock-to-ice ratio in the nucleus. In addition, useful information regarding the formation of the solar system is provided.

Evans, L. G.↗
NASA NTRS1986

VLBI observations of 416 extragalactic radio sources

The Deep Space Network is establishing a high-accuracy Very Long Base Interferometry (VLBI) celestial reference frame. Presented are the VLBI results of observations of 416 radio sources with declination north of -45 degrees which were conducted at frequencies of 2.3 GHz and 8.4 GHz. At 2.3 GHz 323 of 391 radio sources observed were detected with a fringe spacing of 3 milliarcsec and a detection limit of approximately 0.1 Jy. At 8.4 GHz, 278 of 416 radio sources were detected with a fringe spacing of 1 milliarcsec and a detection limit of approximately 0.1 Jy. This survey was conducted primarily to determine the strength of compact components at 8.4 GHz for radio sources previously detected with VLBI at 2.3 GHz. Compact extragalactic radio sources with strong correlated flux densities at both frequencies are used to form a high-accuracy reference frame.

Morabito, D. D.↗
NASA NTRS1986

VLBI observations of 416 extragalactic radio sources

Very long baseline interferometry (VLBI) observations of 416 radio sources with declinations north of -45 deg have been conducted at frequencies of 2.3 and 8.4 GHz. At 2.3 GHz, 323 of 391 radio sources observed were detected with a fringe spacing of 3 milliarcsec and a detection limit of about 0.1 Jy. At 8.4 GHz, 278 of 416 radio sources were detected with a fringe spacing of 1 milliarcsec and a detection limit of about 0.1 Jy. This survey was conducted primarily to determine the strength of compact components at 8.4 GHz for radio sources previously detected with VLBI at 2.3 GHz. Compact extragalactic radio sources with strong correlated flux densities at both frequencies are used to form a high-accuracy reference frame.

Morabito, D. D.↗
NASA NTRS1991

A statistical analysis of gamma-ray bursts detected by the Konus Experiment on Venera 11 and 12

We discuss the advantages of using the V/V sub max method to test well-defined samples of gamma-ray bursts for the spatial uniformity of their parent population. We have applied the V/V sub max test to gamma ray bursts of duration longer than 1 second recorded by the Konus experiment aboard Venera 11 and 12. Based on a sample of 123 bursts, we find V/V sub max equals 0.46 plus or minus 0.03, consistent with a uniform distribution in space. We urge that experimenters give careful attention to the detection limit for each recorded gamma ray burst, and that quantitative data for burst properties and detection limits be published.

Schmidt, Maarten↗
NASA NTRS2024

Launch Complex 39B, SWMU 009, 2023 Performance Monitoring and Air Sparge Expansion Construction Completion Report, Kennedy Space Center, Florida

The 2023 Performance Monitoring and Construction Completion Report (PM-CCR) presents the findings, observations, and results for Air Sparging (AS) operations and expansion activities, as well as sitewide groundwater monitoring for Launch Complex 39B (LC39B), Solid Waste Management Unit (SWMU) 009, at Kennedy Space Center (KSC), Florida. The reporting period for activities covered under this PM-CCR is from January 1, 2023, to December 31, 2023. At LC39B, AS operations began in 2017 in the area west of the launch pad, in the liquid oxygen (LOX) tank area located northwest of the launch pad, and in an area outside of the perimeter fence to protect nearby Outstanding Florida Waters (OFW). The LC39B AS system was installed with 279 AS wells to depths ranging from 23 to 60 feet below land surface (bls), including the sump, correlating to top of screen depths ranging from 20 to 57 feet bls. In December 2022, a total of 22 AS wells were abandoned to support launch pad crane operations, and in November 2023, the system was expanded with five additional AS wells installed to 13 or 17 feet bls near the LOX tank. The remedial objective of the LC39B AS Interim Measure (IM) is to actively decrease concentrations of contaminants of concern (COCs) in groundwater, specifically trichloroethene (TCE), cis-1,2-Dichloroethene (cDCE), and vinyl chloride (VC), to less than their respective Natural Attenuation Default Concentrations (NADCs), so LC39B can transition into a Long-Term Monitoring (LTM) program. This PM-CCR presents the following information for LC39B: • AS system operations and maintenance (O&M) (Year 7 of operation) from January 2023 to December 2023, to include AS trailer relocation in March 2023 and subsequent replacement and re-start in June 2023. • Construction completion details for AS system expansion, which included installation of five new AS wells and one new monitoring well in November 2023. As part of expansion activities, soil samples were also collected for petroleum analysis; no exceedances were identified, and no further investigation for petroleum is warranted. • Performance monitoring results for groundwater sampling events conducted in May/June 2023 (30 wells) and November 2023 (31 wells) in the AS IM area and in the Low Concentration Plume (LCP) areas located north and east of the launch pad for volatile organic compound (VOC) analysis. • Sampling results for one monitoring well, LOX-IW0012S, which is sampled for aluminum on an annual basis (May/June 2023). This well was resampled in November 2023 for both total and dissolved aluminum. Due to a communication error with the laboratory, the May/June 2023 sample was analyzed for total aluminum only. • Groundwater sampling results for per- and polyfluoroalkyl substances (PFAS) collected from seven monitoring wells during the May/June 2023 event to further investigate the Former Sewage Treatment Plant #6 and Percolation Pond area, west of the launch pad. O&M and performance monitoring results show that the AS system at LC39B is operating as designed and meeting performance criteria. Overall runtime was 45 percent (%) during the reporting period (January to December), but the operational runtime was 78% during the timeframe when the system could run (June to December). The most significant downtime contributor was post-launch crane operations following the Artemis launch on November 16, 2022, which lasted until June 2023. During that timeframe, the AS trailer at LC39B was relocated to another KSC remediation site (Wilson Corners) and was subsequently replaced with the AS trailer from the Paint & Oil Locker (POL) remediation site at KSC to resume AS system operations. Performance monitoring results in the AS IM and LCP areas continue to show reduction in COC concentrations over time when compared to baseline levels. In 2023, only one monitoring well (MW0048) detected a COC exceeding its NADC (VC at 740 micrograms per liter [µg/L]), which marks the baseline result for this new well installed during system expansion. Across the rest of the site, VC concentrations have declined or remained stable during the 2023 sampling events. Excluding MW0048, the highest VC result in 2023 was during the May/June sampling event with a concentration of 63 µg/L at MW0032, which is located near MW0048 and the AS expansion area by the LOX tank. TCE was detected in select monitoring wells in the IM area in 2023, but only two locations exceeded the State of Florida Groundwater Cleanup Target Level (GCTL): MW0032 (21 µg/L in May/June 2023 and 9.1 µg/L in November 2023) and MW0036 (5.0 µg/L in November 2023). MW0036 is also located near the LOX tank, on the north side, where the AS system is still operational (Zone Z4). cDCE and trans-1,2-dichloroethene concentrations were less than laboratory method detection limits or their respective GCTLs in all wells sampled in 2023. Near the OFW located northwest of the launch complex, all COC concentrations were less than laboratory method detection limits from monitoring wells (MW0039, MW0040, and LOXTA0002S) sampled in 2023. Aluminum results from LOX-IW0012S, which has been sampled routinely since 2006, detected a total aluminum concentration of 3,900 µg/L during the May/June 2023 sampling event. Results from the November 2023 event detected 5,700 µg/L for total aluminum and 5,500 µg/L for dissolved aluminum. These concentrations slightly decreased from the previous year but remain relatively consistent with historical detections. Aluminum will continue to be sampled on an annual basis at this well as results still exceed the GCTL of 200 µg/L and the Upper Limit of the KSC Background Concentration of 280 µg/L. PFAS results detected nine different PFAS compounds (out of 32 analyzed) from seven wells sampled. Two PFAS compounds, perfluorooctanesulfonic acid (PFOS) and perfluorooctanoic acid (PFOA), currently have FDEP Provisional GCTLs of 70 nanograms per liter (ng/L). All seven samples collected resulted in concentrations less than the FDEP Provisional GCTLs for both PFAS compounds; no exceedances were observed. PFOS and PFOA also have assigned United States Environmental Protection Agency (USEPA) Maximum Contaminant Levels (MCLs) of 4 nanograms per liter (ng/L). None of the PFOS results exceeded the USEPA MCLs. PFOA was detected in two samples above the USEPA MCL at concentrations of 5.8 ng/L (ECS-IW0009I) and 5.5 ng/L (ECS-IW0009S). Three other PFAS compounds, perfluorohexanesulfonic acid (PFHxS), perfluoro-n-nonanoic acid (PFNA), and hexafluoropropylene oxide dimer acid (GenX), currently have USEPA MCLs of 10 ng/L. PFHxS, PFNA, and GenX were not detected at concentrations greater than their respective USEPA MCLs in any of the seven wells. PFAS compounds without FDEP Provisional GCTLs or USEPA MCLs were screened against USEPA RSLs. No other detections exceeded their respective USEPA RSLs. Additional PFAS sampling will be conducted as part of a future PFAS Site Assessment. Based on O&M activities and performance monitoring, the following is recommended for LC39B: • Continue with Year 8 AS system operation within Zone Z4, which includes the AS expansion area. Zone Z3, which has been off since 2018, should remain off as no rebound has been observed. Zones Z1 and Z2, which were turned off at the end of 2022, will remain shut down as monitoring well results have consistently been below GCTLs or have low-level detections with stable or decreasing trends (Meeting Minute 2402-M10, Decision 2402-D30). • Continue with performance monitoring in 2024 with the same monitoring well network as 2023, except with the addition of MW0048 in both semi-annual events. Baseline concentrations for this well were collected during the November 2023 performance monitoring event. Semi-annual sampling should be planned for the May 2024 and November 2024 timeframes (Meeting Minute 2402-M10, Decision 2402-D31). • Continue sampling monitoring well, LOX-IW0012S, for aluminum (total and dissolved) on an annual basis in May 2024. It is also recommended to re-develop this well prior to the next sampling event (Meeting Minute 2402-M10, Decision 2402-D32). The above recommendations for LC39B were presented at the February 2024 KSCRT Meeting, with Team consensus reached on the path forward. The contents of this PM-CCR were also presented at this meeting.

Deborah M Wilson↗
NASA NTRS2013

Toxicological Assessment of ISS Air Quality: April - May 2013

A summary of the analytical results from 4 mini-grab sample (mGSCs) collected on ISS and returned aboard 33S is shown in Table 1. Due to the launch delay of the ATV4 resupply mission, monthly samples were reduced in April and May by omitting sampling of the Service Module in order to ensure contingency samplers were available if needed. Complete data tables of all measured concentrations and corresponding T-values based on 180-day SMACs are enclosed. detection limit for all target compounds, except m/p-xylenes and hexachloro-1, 3-butadiene was 0.025 mg/cu m. The detection limit for m/p-xylenes and hexachloro-1, 3-butadiene and all non-target compounds was 0.05 mg/cu m. The average recoveries of the 3 surrogate standards from the mGSCs were as follows: C-13-acetone, 116 +/- 12%; D-5-fluorobenzene, 117 +/- 7%; and D-5-chlorobenzene, 111 +/- 15%. Initial measured sample pressures were between 13.9 and 14.1 psia for all samples, indicating nominal sample collection. A summary of the analytical results from 3 pairs of passive-diffusion formaldehyde badges collected on ISS and returned aboard 33S is also provided in Table 1. In an effort to conserve samples due to the delay of the ATV4 resupply mission, FMK sampling was only conducted in the US Lab in May. Positive control recoveries (1 trip and 2 lab controls) were 79%, 87%, and 116% respectively.

Meyers, Valerie↗
NASA NTRS1985

Collection and analysis of NASA clean room air samples

The environment of the HALOE assembly clean room at NASA Langley Research Center is analyzed to determine the background levels of airborne organic compounds. Sampling is accomplished by pumping the clean room air through absorbing cartridges. For volatile organics, cartridges are thermally desorbed and then analyzed by gas chromatography and mass spectrometry, compounds are identified by searching the EPA/NIH data base using an interactive operator INCOS computer search algorithm. For semivolatile organics, cartridges are solvent entracted and concentrated extracts are analyzed by gas chromatography-electron capture detection, compound identification is made by matching gas chromatogram retention times with known standards. The detection limits for the semivolatile organics are; 0.89 ng cu m for dioctylphlhalate (DOP) and 1.6 ng cu m for polychlorinated biphenyls (PCB). The detection limit for volatile organics ranges from 1 to 50 parts per trillion. Only trace quantities of organics are detected, the DOP levels do not exceed 2.5 ng cu m and the PCB levels do not exceed 454 ng cu m.

Sheldon, L. S.↗
DOE OSTI2021

An improved Method for Determining Transient Fuel Dilution of Oil in an Internal-Combustion Engine Using Laser-Induced Florescence and Multivariate Least Square Calibration

An optical diagnostic, based on laser-induced fluorescence (LIF), has been developed for on-engine measurements of real-time fuel dilution of engine oil or fuel in oil (FIO). Fuel dilution of oil is broadly relevant to advancing engine technology including durability, calibration, and catalyst-system management, and believed to promote destructive stochastic pre-ignition (SPI) during high-load engine operations. While standard (e.g., ASTM D3524-90) methods are not capable of real-time transient measurements, the LIF technique resolves transient dilution on the minutes time scale. We have expanded on our original FIO instrument development by introducing an improved analysis based on multivariate least square chemometrics analysis. The measurement uses a fuel dye (180–1300 parts per million, by mass) and monitors for its presence in the oil using 532 nm excitation and LIF. While the original FIO instrument utilized a two-color ratio method for analysis, the improved chemometric analysis uses the fully resolved LIF dye spectra to provide better predictive FIO accuracy (>92%) over a wide FIO range (1.5–14%) typical of engine application. We also investigate the effect of oil temperature on the LIF signal. Limited engine applications for demonstrating and validating the improved FIO instrument are shown, and the related data used to quantify practical detection limit and sensitivity. The improved analysis is insensitive to laser power fluctuation and change in detector integration time, providing an excellent FIO sensitivity (1–2%) and detection limit (0.01 %FIO) over a wide range of loads and injection timings, illustrating this updated approach to be a promising tool for advancing engine technology.

42 ENGINEERING↗
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 NTRS2004

Detecting Organic Compounds in Martian Soil Analogues Using Gas Chromatography Mass Spectrometry

One of the primary objectives of the 1976 Viking missions was to determine whether organic compounds, possibly of biological origin, were present in the Martian surface soils. The Viking gas chromatography mass spectrometry (GCMS) instruments found no evidence for any organic compounds of Martian origin above a few parts per billion in the upper 10 cm of surface soil [l], suggesting the absence of a widely distributed Martian biota. However, Benner et d. have suggested that significant amounts of non-volatile organic compounds, possibly including oxidation products of bioorganic molecules (e.g. carboxylic acids) would not have been detected by the Viking GCMS [2]. Moreover, other key organic compounds important to biology, such as amino acids and nucleobases, would also likely have been missed by the Viking GCMS as these compounds require chemical derivatization to be stable in a GC column [3]. Recent pyrolysis experiments with a Mars soil analogue that had been innoculated with Escherichia coli bacteria have shown that amino acid decomposition products (amines) and nucleobases are among the most abundant products generated after pyrolysis of the bacterial cells [4,5]. At the part per billion level (Viking GCMS detection limit), these pyrolysis products generated from several million bacterial cells per gram of Martian soil would not have been detected by the Viking GCMS instruments [4]. Analytical protocols are under development for upcoming in situ lander opportunities to target several important biological compounds including amino acids and nucleobases. For example, extraction and chemical derivatization techniques [3] are being adapted for space flight use to transform reactive or fragile molecules that would not have been detected by the Viking GCMS instruments, into species that are sufficiently volatile to be detected by GCMS. Recent experiments carried out at NASA Goddard have shown that using this derivatization technique all of the targeted compounds mentioned above can be separated on a GC column and detected by MS at sub-picomole (< 10(exp -l2 mole) levels. With these methods, the detection limit for amino acids, carboxylic acids and nucleobases is several orders of magnitude more sensitive than the Viking GCMS instruments for these compounds. Preliminary results using this analytical technique on a variety of Martian soil analogues will be presented.

Glavin, D. P.↗