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All sourcesNASA NTRSDOE OSTI
NASA NTRS2013

The Origin of Carbon-bearing Volatiles in Surprise Valley Hot Springs in the Great Basin: Carbon Isotope and Water Chemistry Characterizations

There are numerous hydrothermal fields within the Great Basin of North America, some of which have been exploited for geothermal resources. With methane and other carbon-bearing compounds being observed, in some cases with high concentrations, however, their origins and formation conditions remain unknown. Thus, studying hydrothermal springs in this area provides us an opportunity to expand our knowledge of subsurface (bio)chemical processes that generate organic compounds in hydrothermal systems, and aid in future development and exploration of potential energy resources as well. While isotope measurement has long been used for recognition of their origins, there are several secondary processes that may generate variations in isotopic compositions: oxidation, re-equilibration of methane and other alkanes with CO2, mixing with compounds of other sources, etc. Therefore, in addition to isotopic analysis, other evidence, including water chemistry and rock compositions, are necessary to identify volatile compounds of different sources. Surprise Valley Hot Springs (SVHS, 41 deg 32'N, 120 deg 5'W), located in a typical basin and range province valley in northeastern California, is a terrestrial hydrothermal spring system of the Great Basin. Previous geophysical studies indicated the presence of clay-rich volcanic and sedimentary rocks of Tertiary age beneath the lava flows in late Tertiary and Quaternary. Water and gas samples were collected for a variety of chemical and isotope composition analyses, including in-situ pH, alkalinity, conductivity, oxidation reduction potential (ORP), major and trace elements, and C and H isotope measurements. Fluids issuing from SVHS can be classified as Na-(Cl)-SO4 type, with the major cation and anion being Na+ and SO4(2-), respectively. Thermodynamic calculation using ORP and major element data indicated that sulfate is the most dominant sulfur species, which is consistent with anion analysis results. Aquifer temperatures at depth estimated by both dissolved SiO2 and Na-K-Ca geothermometers are in the range of 125.0 to 135.4 C, and higher than the values measured at orifices (77.3 to 90.0 C). CO2 and homologs of straight chain alkanes (C1-C5) were identified in gas samples. Carbon isotope values of alkanes increase with carbon numbers. The C-13 fractionation between CO2 and dissolved inorganic carbon suggests they are out of carbon isotope equilibrium. The hypothesis regarding the formation of carbon-bearing compounds in SVHS may involve two processes: 1) Under high heat flow conditions which are caused by regional faulting and crustal extension, original high molecular weight organic compounds (kerogens) in clay-rich rocks decomposed to generate methane and other alkane homologs. 2) The SVHS area is associated with outflow structures, and distant from the heat source. Anaerobic oxidation of methane (AOM) with sulfate at shallow depth (< 90 C) is suggested as being responsible for the generation of CO2 in SVHS.

Fu, Qi↗
NASA NTRS2017

Test and Analysis of Solid Rocket Motor Nozzle Ablative Materials

Asbestos free solid motor internal insulation samples were tested at the MSFC Hyperthermal Facility. Objectives of the test were to gather data for analog characterization of ablative and in-depth thermal performance of rubber materials subject to high enthalpy/pressure flow conditions. Tests were conducted over a range of convective heat fluxes for both inert and chemically reactive sub-sonic free stream gas flow. Instrumentation included use of total calorimeters, thermocouples, and a surface pyrometer for surface temperature measurement. Post-test sample forensics involved measurement of eroded depth, charred depth, total sample weight loss, and documentation of the general condition of the eroded profile. A complete Charring Material Ablator (CMA) style aero-thermal analysis was conducted for the test matrix and results compared to the measured data. In general, comparisons were possible for a number of the cases and the results show a limited predictive ability to model accurately both the ablative response and the in-depth temperature profiles. Lessons learned and modeling recommendations are made regarding future testing and modeling improvements that will increase understanding of the basic chemistry/physics associated with the complicated material ablation process of rubber materials.

Clayton, J. Louie↗
NASA NTRS2007

NASA GRC and MSFC Space-Plasma Arc Testing Procedures

Tests of arcing and current collection in simulated space plasma conditions have been performed at the NASA Glenn Research Center (GRC) in Cleveland, Ohio, for over 30 years and at the Marshall Space Flight Center (MSFC) in Huntsville, Alabama, for almost as long. During this period, proper test conditions for accurate and meaningful space simulation have been worked out, comparisons with actual space performance in spaceflight tests and with real operational satellites have been made, and NASA has achieved our own internal standards for test protocols. It is the purpose of this paper to communicate the test conditions, test procedures, and types of analysis used at NASA GRC and MSFC to the space environmental testing community at large, to help with international space-plasma arcing-testing standardization. Discussed herein are neutral gas conditions, plasma densities and uniformity, vacuum chamber sizes, sample sizes and Debye lengths, biasing samples versus self-generated voltages, floating samples versus grounded samples, test electrical conditions, arc detection, preventing sustained discharges during testing, real samples versus idealized samples, validity of LEO tests for GEO samples, extracting arc threshold information from arc rate versus voltage tests, snapover, current collection, and glows at positive sample bias, Kapton pyrolysis, thresholds for trigger arcs, sustained arcs, dielectric breakdown and Paschen discharge, tether arcing and testing in very dense plasmas (i.e. thruster plumes), arc mitigation strategies, charging mitigation strategies, models, and analysis of test results. Finally, the necessity of testing will be emphasized, not to the exclusion of modeling, but as part of a complete strategy for determining when and if arcs will occur, and preventing them from occurring in space.

Ferguson, Dale C.↗
NASA NTRSDate not supplied

Laboratory Investigation of the Effect of Venusian Weathering on Mineral Spectra

Introduction: The recent selection of two missions to Venus has renewed the importance of deter-mining weathering reactions between minerals and the Venusian atmosphere, and the spectral signatures of minerals before, during, and after these reactions. The rate at which weathering reactions progress also constrain show long unstable minerals will be present on the surface (e.g., [1]), and enables the use of mineralogy as a constraint on surface age(e.g., [2-3]).In order to gain an understanding of how mineral compositions and spectra change with weathering, we have begun conducting experiments in a 1 atm experimental setup at Wesleyan University. This setup exposes minerals to the temperature and most abundant gases of the Venus atmosphere (CO2, SO2, N2).We conducted initial experiments using biotite, calcite, and montmorillonite in order to test our methodology with minerals that may be relevant to recording the history of water on Venus. Methods: Experiments were conducted in Thermo Fisher Scientific Lindberg/Blue M Mini-Mite horizontal tube furnaces at Wesleyan University. Experiments used natural mineral chips and powders, and were conducted at 1 atmosphere and 460 °C under pre-mixed gases provided by Air Gas(Table 1). The furnaces are set up in a flow through configuration so that solid samples are exposed to a fixed gas composition, and quartz glass process tubes were used in all experiments (1/4” diameter for experiment V4, ½” diameter for all others). These conditions were maintained for the du-rations listed in Table 1, at which point the furnace was turned off with gas flowing until the sample was cool enough to extract under N2and be placed in a desiccator for storage. Run products were carbon coated and examined using a Hitachi SU5000 Field Emission Gun Scanning Electron Microscope (SEM) equipped with an EDAX Octane Pro EDS detector located at Wesley-an University. Visible-Near Infrared Spectroscopy (VNIR) analysis was performed on powdered samples under a nitrogen atmosphere using an ASD Fieldspec Proover the 350-2500 nm range. Powdered mineral samples were milled to a particle size of < 45μm and were spiked with an internal standard (Al2O3, corundum) to obtain quantitative mineralogy. Samples were analyzed using a Panalytical X’Pert pro X-ray Diffractometer (XRD), with an X’Celerator high speed detector and Co Kα radiation, with data collected at a step size of 0.02 ̊/minute step counting rate from 2 to 80 degrees 2θ at 45 mA/40kV in the X-ray Diffraction Laboratory located at NASA Johnson Space Center. Materials Data Inc (MDI) software suite, JadeTMv9 was used for Rietveld refinement to determine phase abundances and mineral identification by comparing XRD patterns to International Center for Diffraction Data (ICDD) database patterns. Table 1: Experimental matrix. Experiment Name Duration (Days)Gas Com-position (trace gas)MineralsV487SO2/N2(1.4%)Montmorillonite, biotiteV519SO2/N2(1.4%)CalciteV619CO2/SO2/N2(1.4% SO2, 2.1% N2)Montmorillonite, biotiteV828SO2/N2(1.4%)Biotite, calcite Results: Calcite. In both experiments, calcite was exposed to the SO2/N2gas mixture, and in both experimental run products, XRD analysis detected anhydrite, which is consistent with EDS measurements conducted in the SEM. The XRD analyses show greater amounts of anhydrite present after 28 days than 19, suggesting the calcite reaction progressed further given longer duration. Grain surface morphology as seen in the SEM also shows secondary mineral growth (Fig. 1). VNIR spectra show no change, as expected since anhydrite lacks spectral features in this wavelength range. Montmorillonite. Montmorillonite was exposed to two different gas mixtures, the SO2/N2mix and CO2/SO2/N2mix over different durations (87 and 19 days, respectively). VNIR analyses of both run products show a reduction in the 1441and1910 nm water features as well as a shift of the 1411 and 2011 nm features to shorter wavelengths that may indicate re-structuring in the crystal lattice and the production of amorphous phases [4]. XRD results are consistent with this, showing a shift of the 001 peak from 15Åto 10Åin both run products. The amount of X-ray amorphous material in the montmorillonite run products was greater than that present in the unreacted clay, being the greatest in the 87 day V4 experiment. No other secondary phases were detected in the run products, however sulfur was present in EDS analyses of powder samples.

A R Santos↗
DOE OSTI2018

Effect of laser power on oxygen and nitrogen concentration of commercially pure titanium manufactured by selective laser melting

Highlights: • The hardness and strength of pure titanium fabricated by SLM were increased with increasing the laser power. • During the SLM processing, the concentrations of oxygen and nitrogen in the SLM parts were increased. • The oxidation and nitriding were thermodynamically possible under SLM. - Abstract: This study analyzed the variation of mechanical properties and its causes with increasing the laser power in the fabrication of pure titanium by selective laser melting (SLM). SLM samples were fabricated using commercially pure titanium grade 1 powder when the scan speed was 1000 mm/s and the laser power as 120, 200, 280, 360, and 440 W, respectively. As the laser power increased, the hardness and strength of the samples increased gradually. During the SLM processing, the concentrations of oxygen and nitrogen in the SLM samples were increased, which resulted in the increase of hardness and strength. The SLM equipment used in this study removed oxygen in the chamber by flowing high purity argon gas and fabricates the sample while preserving the oxygen concentration in the atmosphere to 0.2%. Evaluating the possibility of oxidation and nitriding during the SLM process by thermodynamic analysis, it was found that the process occurred under conditions in which temperature and residual oxygen and nitrogen partial pressure led to oxidation and nitriding.

36 MATERIALS SCIENCE↗
NASA NTRS1977

Portable mass spectrometer

Eighteen-pound unit gives real-time onsite sample analysis. Mass range is twelve to two hundred atomic mass units with resolution of two hundred. Device has biomedical application possibilities, such as determination of alcohol and gas content of blood and breath.

Giffin, C. E.↗
NASA NTRS1993

Thermal Analyzer for Planetary Soil (TAPS): an in Situ Instrument for Mineral and Volatile-element Measurements

Thermal Analyzer for Planetary Soil (TAPS) offers a specific implementation for the generic thermal analyzer/evolved-gas analyzer (TA/EGA) function included in the Mars Environmental Survey (MESUR) strawman payload; applications to asteroids and comets are also possible. The baseline TAPS is a single-sample differential scanning calorimeter (DSC), backed by a capacitive-polymer humidity sensor, with an integrated sampling mechanism. After placement on a planetary surface, TAPS acquires 10-50 mg of soil or sediment and heats the sample from ambient temperature to 1000-1300 K. During heating, DSC data are taken for the solid and evolved gases are swept past the water sensor. Through ground based data analysis, multicomponent DSC data are deconvolved and correlated with the water release profile to quantitatively determine the types and relative proportions of volatile-bearing minerals such as clays and other hydrates, carbonates, and nitrates. The rapid-response humidity sensors also achieve quantitative analysis of total water. After conclusion of soil-analysis operations, the humidity sensors become available for meteorology. The baseline design fits within a circular-cylindrical volume less than 1000 cm(sup 3), occupies 1.2 kg mass, and consumes about 2 Whr of power per analysis. Enhanced designs would acquire and analyze multiple samples and employ additional microchemical sensors for analysis of CO2, SO2, NO(x), and other gaseous species. Atmospheric pumps are also being considered as alternatives to pressurized purge gas.

Gooding, J. L.↗
NASA NTRS2010

VAPoR - Volatile Analysis by Pyrolysis of Regolith - an Instrument for In Situ Detection of Water, Noble Gases, and Organics on the Moon

We present the Volatile Analysis by Pyrolysis of Regolith (VAPoR) instrument design and demonstrate the validity of an in situ pyrolysis mass spectrometer for evolved gas analyses of lunar and planetary regolith samples. In situ evolved gas analyses of the lunar regolith have not yet been carried out and no atmospheric or evolved gas measurements have been made at the lunar poles. VAPoR is designed to do both kinds of measurements, is currently under development at NASA's Goddard Space Flight Center, and will be able to heat powdered regolith samples or rock drill fines up to 1400 C in vacuo. To validate the instrument concept, evolved gas species released from different planetary analogs were determined as a function of temperature using a laboratory breadboard. Evolved gas measurements of an Apollo 16 regolith sample and a fragment of the carbonaceous meteorite Murchison were made by VAPoR and our results compared with existing data. The results imply that in situ evolved gas measurements of the lunar regolith at the polar regions by VAPoR will be a very powerful tool for identifying water and other volatile signatures of lunar or exogenous origin as potential resources for future human exploration.

ten Kate, I. L.↗
NASA NTRS2011

Synthesis of Stacked-Cup Carbon Nanotubes in a Metal Free Low Temperature System

Stacked-cup carbon nanotubes were formed by either Fischer-Tropsch type or Haber Bosch type reactions in a metal free system. Graphite particles were used as the catalyst. The samples were heated at 600 C in a gas mixture of CO 75 Torr, N2 75 Torr and H2 550 Torr for three days. Trans mission electron microscope analysis of the catalyst surface at the completion of the experiment recognized the growth of nanotubes. They were 10-50 nm in diameter and approximately 1 micrometer in length. They had a hollow channel of 5-20 nm in the center. The nanotubes may have grown on graphite surfaces by the CO disproportionation reaction and the surface tension of the carbon nucleus may have determined the diameter. Although, generally, the diameter of a carbon nanotube depends on the size of the cataly1ic particles, the diameter of the nanotubes on graphite particles was independent of the particle size and significantly confined within a narrow range compared with that produced using catalytic amorphous iron-silicate nanoparticles. Therefore, they must have an unknown formation process that is different than the generally accepted mechanism.

Kimura, Yuki↗
NASA NTRS2016

Mapping of Spacecraft Atmosphere Monitor Signal to Major Constituent Abundances

The Spacecraft Atmosphere Monitor (S.A.M.) follows the JPL’s commitment to introduce and develop next-generation instrumentation concepts for sensing the air quality on manned space flights via continuous sampling, measuring, and reporting in 2s intervals on all gaseous pollutants. The S.A.M. will have two modes of operation: the Major Constituent Analysis (MCA) mode and the Trace Gas Analysis (TGA) mode. The MCA mode will report on molecular analytes such as CH4, H2O, N2, O2, Ar, and CO2 while the TGA mode will acquire minute amounts of volatile organic compounds. Both modes assess the composition of the ambient air with twenty full mass spectra per second giving rise to a substantial amount of data to be processed by a set of small footprint software stacks hosted by an on-board computer. Mass spectra will be accumulated as the number of counts recorded in a given mass-to-charge channel and converted into the absolute abundances of detected species using an efficient algorithm. The decomposition algorithm contains four units: peak identification, mass calibration, background and dead time correction, and an abundance analysis unit. The abundance analysis module identifies target species through their characteristic fragmentation patterns in the presence of molecular isobars, such as CO and N2. For example, in order to identify N2 analyte, the code will simultaneously monitor abundance ratios of the 14, 28 and 29 Th signals and will adapt to any instability caused by a decrease in ambient pressure or changes in humidity. This requirement becomes critical for instruments designed to monitor the near real-time quality of cabin air and promptly provide accurate feedbacks.

Nikolic, D.↗
DOE OSTI2024

Sub-Diurnal Methane Variations on Mars Driven by Barometric Pumping and Planetary Boundary Layer Evolution

In recent years, the Tunable Laser Spectrometer within the Sample Analysis at Mars (TLS-SAM) instrument on board the Mars Science Laboratory (MSL) Curiosity rover has detected methane variations in the atmosphere at Gale crater. Methane concentrations appear to fluctuate seasonally as well as sub-diurnally, which is difficult to reconcile with an as-yet-unknown transport mechanism delivering the gas from underground to the atmosphere. To potentially explain the fluctuations, we consider barometrically induced transport of methane from an underground source to the surface, modulated by temperature-dependent adsorption. The subsurface fractured-rock seepage model is coupled to a simplified 1-D atmospheric mixing model to provide insights on the pattern of atmospheric methane concentrations in response to transient surface methane emissions, as well as to predict sub-diurnal variation in methane abundance for the northern summer period, which is a candidate time frame for a MSL Curiosity sampling campaign. Our analysis suggests that there is a lower limit to the subsurface fracture density that can produce the observed methane patterns, below which the atmospheric methane variations would be out of phase with the observations. The best-performing model scenarios indicate a significant, short-lived methane pulse just prior to sunrise, the detection of which by TLS-SAM would be a potential indicator of the contribution of barometric pumping to Mars' atmospheric methane variations.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS2015

Time‐Series Analysis: A Cautionary Tale

Time-series analysis has often been a useful tool in atmospheric science for deriving long-term trends in various atmospherically important parameters (e.g., temperature or the concentration of trace gas species). In particular, time-series analysis has been repeatedly applied to satellite datasets in order to derive the long-term trends in stratospheric ozone, which is a critical atmospheric constituent. However, many of the potential pitfalls relating to the non-uniform sampling of the datasets were often ignored and the results presented by the scientific community have been unknowingly biased. A newly developed and more robust application of this technique is applied to the Stratospheric Aerosol and Gas Experiment (SAGE) II version 7.0 ozone dataset and the previous biases and newly derived trends are presented.

Damadeo, Robert↗
NASA NTRS2003

Sample Analysis at Mars

The next landed missions to Mars, such as the planned Mars Science Laboratory and ExoMars, will require sample analysis capabilities refined well beyond what has been flown to date. A key science objective driving this requirement is the determination of the carbon inventory of Mars, and particularly the detection of organic compounds. While the gas chromatograph mass spectrometers (GC/MS) on the Viking landers did not detect any indigenous organics in near surface fines, it is possible that these measurements were not representative of Mars on the whole. That is, those compounds to which the GC/MS was sensitive would likely not have survived the strong oxidative decomposition in the regolith at the landing sites in question. The near surface fines could very well contain a significant quantity of refractory compounds that would not have been volatilized in the sample ovens on Viking. It is also possible that volatile organics exist on Mars in sedimentary, subsurface, or polar niches.

W B Brinckerhoff↗
NASA NTRS2003

Sample Analysis At Mars

The next landed missions to Mars, such as the planned Mars Science Laboratory and ExoMars, will require sample analysis capabilities refined well beyond what has been flown to date. A key science objective driving this requirement is the determination of the carbon inventory of Mars, and particularly the detection of organic compounds. While the gas chromatograph mass spectrometers (GCMS) on the Viking landers did not detect any indigenous organics in near surface fines, it is possible that these measurements were not representative of Mars on the whole. That is, those compounds to which the GC/MS was sensitive would likely not have survived the strong oxidative decomposition in the regolith at the landing sites in question. The near surface fines could very well contain a significant quantity of refractory compounds that would not have been volatilized in the sample ovens on Viking. It is also possible that volatile organics exist on Mars in sedimentary, subsurface, or polar niches.

Brinckerhoff, W. B.↗
DOE OSTI2020

Complete Round-Robin Hydrogen Gas Analysis Capability Comparison (Milestone 2.6)

The Department of Energy (DOE) is currently evaluating strategies for the extended dry storage of aluminum-clad spent nuclear fuel (ASNF). Part of this assessment concerns the extent of radiolytic molecular hydrogen (H2) generation from the aluminum cladding’s oxyhydroxide corrosion layers. Understanding this radiation-induced process and the factors effecting it (e.g., system conditions such as temperature and gaseous environment) are essential for the development of predictive computer models to support the Technical Considerations and Challenges for Extended (> 50 yrs) Dry Storage of ASNF program. To achieve this goal and ensure that the experimental data gathered by Task 2 (Oxyhydroxide Layer Radiolytic Gas Generation Resolution) research groups (Idaho National Laboratory and Savannah River National Laboratory) are consistent, a round-robin H2 analysis capability comparison was initiated. Here we present the results from said round-robin and conclude that despite differences in sample preparation, irradiation parameters, and analytical procedures, the measured data are sufficiently consistent between the two laboratories (= 15%).

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗
NASA NTRS2024

Xenon Isotopic Analysis of Individual Intermediate Particles From the OSIRIS-REx Sample of Asteroid Bennu

The OSIRIS-REx mission sampled material from the B-type asteroid Bennu and delivered the sample to Earth on 24 September 2023. Here we present initial xenon isotopic analysis of individual intermediate particles of Bennu material collected by the OSIRIS-REx mission. Noble gases are key tracers of Solar System evolution. Xenon is particularly useful among the noble gases because its nine isotopes allow multiple contributing sources to be unambiguously identified. The sun, asteroids (as measured in meteorites), and comets (measured in the coma of comet 67P) have distinct xenon isotopic signatures reflecting different mixtures of nucleosynthetic components. In addition, 129 I, 238 U, and 244 Pu decay with different half-lives, producing characteristic xenon signatures. Exposure of samples containing light rare earth elements and barium to cosmic rays produces xenon from spallation and secondary neutron capture reaction. Noble gas analyses help address several of the driving hypotheses of the mission [9]. Particle-by-particle analysis can elucidate the diversity of material present and reveal distinct noble gas compositions, including the potential to detect presolar or cometary noble gas signatures on a small scale. The isotopic signature provides a fingerprint that can be used to constrain the sources of volatiles in planetary reservoirs and combined with other information (e.g. mineralogy and petrology of the material analyses) contributes to our understanding of the initial constituents, formation, and history of Bennu and its parent asteroid.

S A Crowther↗
DOE OSTI2018

UV-filters and musk fragrances in seafood commercialized in Europe Union: Occurrence, risk and exposure assessment

Highlights: • Largest survey on UV-Fs and musks in seafood commercialized in Europe. • Farmed seabream showed the highest average concentration of UV-Fs. • Wild mackerel showed the highest average concentration of polycyclic musks. • UV-Fs and musks in raw samples were far below the estimated toxicological reference value. In the framework of the FP7 ECsafeSeafood project, 62 seafood samples commercialized in Europe Union from several representative species – mackerel, tuna, salmon, seabream, cod, monkfish, crab, shrimp, octopus, perch and plaice – were analysed for residues of 21 personal care products (PCPs), including 11 UV-filters (UV-Fs) and 10 musk fragrances (musks). PCPs analysis were performed by Quick, Easy, Cheap, Effective Rugged, Safe (QuEChERS), combined with liquid-liquid extraction (LLE) or dispersive solid-phase extraction (dSPE), followed by gas chromatography-tandem mass spectrometry (GC-MS/MS). The results showed the presence in a wide range of samples of nine out of eleven UV-Fs compounds analysed, namely 2-ethylhexyl salicylate (EHS), 2-ethylhexyl,4-methoxycinnamate (EHMC), 4-methylbenzylidenecamphor (4-MBC), benzophenone-1 (BP1), benzophenone-3 (BP3), isoamyl-4-methoxycinnamate (IMC), 2,2′-dihydroxy-4,4′-dimethoxybenzophenone (DHMB), homosalate (HS), and octocrylene (OC), whereas galaxolide (HHCB), galaxolide lactone (HHCB-lactone), and tonalide (AHTN) were the most found musks. The potential risks to human health associated with the exposure to eight of the more prevalent PCPs – EHS, EHMC, 4-MBC, BP1, BP3, IMC, HHCB, and AHTN - through seafood consumption were assessed for consumers from five European countries (Belgium, Ireland, Italy, Portugal and Spain). Results showed that the human exposure to UV-Fs and musks estimated from the concentration values found in seafood and the daily consumption of concerned seafood species, were far below toxicological reference values.

54 ENVIRONMENTAL SCIENCES↗
DOE OSTI2019

Impact of Lubricant Oil Additives on the Performance of Pd-Based Three-Way Catalysts

As alternative lubricant anti-wear additives are sought to reduce friction and improve overall fuel economy, it is important that these additives are also compatible with current emissions control catalysts. In the present work, a second-generation oil-miscible phosphorous-containing ionic liquid (IL), is evaluated for its impact on Pd-based three-way catalyst (TWC) reactivity and benchmarked against the industry standard zinc dialkyl-dithio-phosphate (ZDDP). The TWCs are exposed to the lubricant additives in an engine bench under four different scenarios: base case with no additive (NA), ZDDP-only, IL-only, and IL + ZDDP. The engine-aged TWC samples, along with the as-received TWC, are characterized through various analytical techniques including catalyst reactivity evaluation in a bench-flow reactor. The temperature of 50% conversion (T 50 ) for the ZDDP-aged TWC increases by 11, 21, and 36 °C for CO, C 3 H 6 , and C 3 H 8 , respectively, as compared with the no-additive case. Similarly, the T50 for IL-only and IL + ZDDP-aged TWCs also increase as compared with the no-additive case. Even though the water-gas-shift (WGS) reactivity is similar for all engine-aged samples, the IL-aged TWC had higher oxygen storage capacity than the ZDDP-aged TWC. EPMA analysis reveals penetration of phosphorus deep into the washcoat for all engine-aged TWCs. Results from XRD indicate the presence of CePO 4 and AlPO 4 on the washcoat of IL, ZDDP, and IL + ZDDP-aged TWC samples but not on the fresh and NA TWC samples. Additionally, ICP-OES results show a large amount of phosphorus in the washcoat of IL, ZDDP and IL + ZDDP-aged TWC samples and a lesser amount in NA TWC samples.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗